Day: October 16, 2020

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 24621-61-2,(S)-Butane-1,3-diol, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.24621-61-2

Example 63 (R)-3- {2-CHLORO-4- [3- (4-CHLORO-2-PHENOXY-PHENOXY)-BUTOXY]-PHENYL}-PROPIONIC acid Step A (S) -Acetic acid 3-hydroxy-butyl ester; A mixture of (S)- (+)-1, 3-butanediol (10.0 g, 0.1 mol) and 2,4, 6-collidine (27 g, 0.2 mol) in DCM (100 mL) is cooled to-78 C. The reaction is then treated dropwise with acetyl chloride (10.4 g, 0.13 mol), and stirred for 2hr AT-78 C. The reaction is then allowed to warm to rt and stir for an additional hour. The reaction is then quenched with IN HCl and extracted with DCM. The organic layer is separated, washed with brine, and dried over NA2SO4. The organic is filtered, and the solvent is removed to afford 9.77 g (66%) of acetic acid 3-hydroxy-butyl ESTER. IH NMR (400 MHz, CDC13) ; MS (ES+) NILZ mass calcd for C6HI203 132, found 133 (M + 1).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. (S)-Butane-1,3-diol, We look forward to the emergence of more reaction modes in the future.

Reference£º
Patent; ELI LILLY AND COMPANY; WO2005/19151; (2005); A1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

24621-61-2, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact.24621-61-2,(S)-Butane-1,3-diol, it is a common compound, a new synthetic route is introduced below.

Production of (S)-3-Hydroxy-1-(p-toluenesulfonyloxy)butane In the same manner as in the first step of Production Example 32, the desired compound (77.5 g) was obtained as light brown oil from (S)-1,3-butanediol (30.0 g) and p-toluenesulfonyl chloride (69.8 g). The thus-obtained oil was immediately subjected to the next step., 24621-61-2

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 24621-61-2, other downstream synthetic routes, hurry up and to see.

Reference£º
Patent; Fujisawa Pharmaceutical Co., Ltd.; US6420409; (2002); B1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 24621-61-2,24621-61-2

p-Toluenesulfonyl chloride (381 mg, 1 .68 mmol) was dissolved in anhydrous DCM (10 mL) at RT under N2. (s)-(+)-1 ,3-butandiol (300 muIota_, 3.33 mmol) was added followed by NEt3 (450 muIota_, 3.33 mmol) and the solution stirred for 18 h. The solution was partitioned with H2O (15 mL) and extracted with DCM (3 x 10 mL), Combined organic fractions were dried by phase separator and the mixture loaded onto silica for purification by flash chromatography. The desired compound A32 was isolated as a clear oil (144 mg, 29%); -NMR (400 MHz, DMSO-c/6): delta 7.78 (d, J = 8.0 Hz, 2H), 7.48 (d, J = 8.0 Hz, 2H), 4.56 (d, J = 5.0 Hz, 1 H), 4.12-4.00 (m, 2H), 3.65-3.57 (m, 1 H). 2.43 (s, 3H), 1 .69-1 .54 (m, 2H), 1 .00 (d, J = 6.0 Hz, 3H).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 24621-61-2.

Reference£º
Patent; IMPERIAL INNOVATIONS LIMITED; SCHNEIDER, Michael; NEWTON, Gary; CHAPMAN, Katie; PERRIOR, Trevor; JARVIS, Ashley; LOW, Caroline; AQIL, Rehan; FISHER, Martin; BAYFORD, Melanie; CHAPMAN, Nicholas; MARTIN, Nicholas; REISINGER, Tifelle; NEGOITA-GIRAS, Gabriel; (260 pag.)WO2019/73253; (2019); A1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

24621-61-2,Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.24621-61-2,A new synthetic method of this compound is introduced below.

To a solution of (S)+}1,3-butanediol (10.0 g, 0.110 mol), was added triphenylmethylchloride (33.0 g, 0.330 mol), 4-dimethylaminopyridine (1.40 g, 11.5 mmol) in CH2Cl/pyridine (1:1, 500 mL).Stirring was continued over 48 h. The solvent was removed, the mixture was diluted with ether, washed with brine and dried over Na2SO4. The organic solution was filtered and concentrated. Silica gel chromatography with (5% ethyl acetate/hexanes) produced a clear oil (24 g) in 70% yield.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, (S)-Butane-1,3-diol.

Reference£º
Patent; Bristol-Myers Squibb Company; Merck & Co. Inc.; US6967196; (2005); B1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 538-58-9,538-58-9

General procedure: A mixture of unsaturated ketone 1a (60.7 mg, 0.25 mmol) and phosphonium salt 2a (198.6 mg, 0.45 mmol) in CH3CN (2 mL) was stirred for 5 min. Then DBU (127 muL) in CH3CN (0.5 mL) was added. The reaction mixture was stirred at 60 C for 6 h and then air was introduced with a balloon for another 42 h. After the reaction was completed, the reaction mixture was filtered through a short silica gel column and washed with DCM. The filtrate was concentrated under reduced pressure and the residue was purified by flash chromatography (PE/EtOAc, 60/1) to afford 3a as a colorless oil (69.3 mg, 86% yield).

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 538-58-9.

Reference£º
Article; Shu, Zhen-Cao; Zhu, Jian-Bo; Liao, Saihu; Sun, Xiu-Li; Tang, Yong; Tetrahedron; vol. 69; 1; (2013); p. 284 – 292;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 19132-06-0,(2S,3S)-Butane-2,3-diol, as follows.19132-06-0

To a 500-mL, 3-necked round-bottomed flask (equipped with a water- cooled reflux condenser and an HCI trap) was added (2s,3s)-(-f-)-2.3-butanediol (Aldrich, Milwaukee Wisconsin)(1500 nil, 166 mniol) and CCI4 (120 ml). Thionyl chloride. reagentplus (14.57 ml, 200 mmoi) was then added drop wise viaa syringe over a period of 20 minutes and the resulting mixture was heated to98 C for 45 minutes, then it was allowed to cool to room temperature. Rf ofintermediate == 0.42 eluting with 50% EtOAc in heptanes; use KMNO4 to visualizecompound, The reaction mixture was then cooled in an ice-water bath. MeCN(120 mL) and water (150 rnL) were added followed by ruthenium(111) chloride(0.035g. 0.166 nunol). Sodium periodate (53.4 g, 250 rnmol) was then addedslowly portion wise over 30 minutes. The resulting biphasic brown mixture was stirred vigorously whie allowed to reach room temperature for a period of 1.5 hour (internal temperature never increased above room temperature). TLC (50% EtOAc in heptanes) showed complete conversion. The crude mixture was thenpoured into ice water and extracted twice with 300 ml of diethyl ether. The combined organic layers were washed once with 200 ml of saturated sodium bicarbonate, washed once with 200 nil of brine, dried over sodium sulfate and concentrated by rotary evaporation to give (4S.5 S)-4,5-dimethyi- 1,3,2- dioxathiolane 2,2-dioxide (21.2 g, 139 mmoi) as a red oil.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, (2S,3S)-Butane-2,3-diol, and friends who are interested can also refer to it.

Reference£º
Patent; AMGEN INC.; BROWN, Sean P.; BEDKE, David Karl; DEGRAFFENREID, Michael R.; FU, Jiasheng; LI, Zhihong; GONZALEZ LOPEZ DE TURISO, Felix; GONZALEZ BUENROSTRO, Ana; GRIBBLE, Jr., Michael W.; JOHNSON, Michael G.; KOHN, Todd J.; LI, Kexue; LI, Yunxiao; LIZARZABURU, Mike Elias; REW, Yosup; TAYGERLY, Joshua; WANG, Yingcai; YAN, Xuelei; YU, Ming; ZHU, Jiang; ZANCANELLA, Manuel; JIAO, Xian Yun; ZHU, Liusheng; WANG, Xianghong; MEDINA, Julio C.; DUQUETTE, Jason A.; HOUZE, Jonathan B.; VIMOLRATANA, Marc; CARDOZO, Mario G.; CHENG, Alan C.; (2426 pag.)WO2017/147410; (2017); A1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 4254-15-3,(S)-Propane-1,2-diol, as follows.4254-15-3

(1) Feeding800 kg of S-propylene glycol, 1600 kg of dimethyl carbonate and 8 kg of sodium methoxide solution were added to the reaction vessel, and heating and stirring were started.The sodium methoxide solution is a 30percent sodium methoxide/methanol solution;The S-propanediol has a propylene glycol content of 99.5percent, a moisture content of 0.5percent, and a specific rotation of ?16.80-17. (2) Temperature rise reactionFirst stage heating reaction The temperature is raised to 60-65 ¡ã C, at which time a solution (mainly methanol, a small portion of dimethyl carbonate) is distilled off, received in the receiving tank, and the solution is evaporated; Second stage heating reactionThereafter, after about 12 hours, the temperature is raised from 65 ¡ã C to 90 ¡ã C, the solution is kept distilled, and the product is distilled as a by-product alcohol-based fuel (methanol and dimethyl carbonate); Third stage temperature rise reactionHeating was continued, and the temperature was raised from 90 ¡ã C to 115 ¡ã C for 8 hours, and the heating was stopped. (3) Cooling downThe temperature was lowered from 115 ¡ã C to 60 ¡ã C. The temperature in the reaction vessel is ?90 ¡ã C, and the alcohol-based fuel (mixed solution of methanol and dimethyl carbonate) is distilled off; most of the steam distilled out at >90 ¡ã C is dimethyl carbonate, and a small amount of methanol is used as a reaction raw material for recovery. (4) Decompression reaction under reduced pressureStart decompression under reduced pressure, using vacuum distillation, vacuum degree ? -0.08mpa, the temperature rises at a rate of 0.2 ¡ã C per minute,Continue to distill the solution (a mixture of methanol and dimethyl carbonate),Keep the solution evaporated, when the temperature rises to 120 ¡ã C, basically no solvent comes out at this time,The pressure reduction and desolvation can be stopped, and the temperature is lowered; the remaining liquid in the reaction tank is (S)-propylene carbonate. In the crude (S)-propylene carbonate, the (S)-propylene carbonate content is 97percent or more. From the start of the preparation to the preparation of the crude product, the reaction time was 25 hours. (5) Distillation reactionTransfer the remaining liquid after decompression and decompression to the rectification bottle, and turn on the heating and stirring.Vacuuming, ensuring a vacuum degree ? 0.1Mpa, starting the steaming before the fraction, steaming out about 100kg of the former fraction, and then transferring the finished product.The materials in the rectification tank were all distilled off, the rectification was stopped, and (S)-propylene carbonate was collected. The (S)-propylene carbonate has the following quality indicators:1. Appearance: colorless clear liquid;2, SPC chemical purity content (percent): ? 99.8;3, SPC optical purity content (percent): ? 99.4;4. SPC isomer content (percent): ? 0.6;5. Moisture (percent): ? 0.1; The yield of the finished SPC is 97percent; the specific rotation is -2 to -3;

According to the analysis of related databases, (S)-Propane-1,2-diol, the application of this compound in the production field has become more and more popular.

Reference£º
Patent; Weifang Huitao Chemical Co., Ltd.; Liu Jianwei; Zhang Quansheng; Wei Lanxing; Hua Xian; (6 pag.)CN109369401; (2019); A;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

4254-15-3,Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials.4254-15-3,A new synthetic method of this compound is introduced below.

Example 18C N-[(2Z)-3-butyl[1,3]thiazolo[4,5-c]pyridin-2(3H)-ylidene]-2-{[(2S)-2-hydroxypropyl]oxy}-5-(trifluoromethyl)benzamide (S)-propane-1,2-diol (52 mg, 0.68 mmol) in THF (1 mL) was treated with NaH (60percent dispersion; 27 mg, 0.68 mmol) at room temperature for 20 minutes. The mixture was cooled to 0¡ã C. and a solution of Example 18B (90 mg, 0.23 mmol) in THF (1 mL) was added. The mixture was allowed to warm to room temperature, and stirred for 4 hours. The mixture was diluted with saturated aqueous NaHCO3 (20 mL) and extracted with ethyl acetate (2.x.30 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated. The residue was purified by column chromatography using an Analogix.(R). Intelliflash280.(TM). (SiO2, 0-100percent ethyl acetate in hexanes) to afford 19 mg (19percent) of the title compound. 1H NMR (500 MHz, CDCl3) delta ppm 1.04 (t, J=7.48 Hz, 3H) 1.28 (d, J=6.41 Hz, 3H) 1.47-1.59 (m, 2H) 1.88-1.98 (m, 2H) 3.87 (t, J=8.85 Hz, 1H) 4.21-4.31 (m, 1H) 4.35 (dd, J=9.15, 2.75 Hz, 1H) 4.51-4.59 (m, 2H) 7.12 (d, J=8.85 Hz, 1H) 7.72 (dd, J=8.54, 2.14 Hz, 2H) 8.51 (d, J=1.83 Hz, 2H) 8.75 (s, 1H); MS (DCI/NH3) m/z 454 (M+H)+.

If you are interested in these compounds, you can also browse my other articles.Thank you for taking the time to read this article. I hope you enjoyed it, (S)-Propane-1,2-diol.

Reference£º
Patent; ABBOTT LABORATORIES; US2011/144165; (2011); A1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

The major producers of chemicals have been the Europe, Japan and China. Due to the growing call for a cleaner, greener environment, people will have to find innovative ways to maintain their relevance. Here is a downstream synthesis route of the compound 538-58-9,538-58-9

538-58-9, General procedure: In a general procedure, dibenzylidene acetone (1 mmol), N,N-dimethylbarbituric acid/barbituric acid/thiobarbituric acid(1 mmol) and 4 mL of ethanol:water (1:1) were taken in a 50 mL round-bottomed flask. 10 mol% of tetrabutyl ammonium bromide (TBAB) was added to the mixture, and the contents were stirred. The reaction mixture was refluxed and the progress of the reaction was monitored by TLC using ethyl acetate:petroleum ether (30:70) as eluent for disappearance of active methylene compounds. After completion of the reaction, the reaction mixture was allowed to cool to room temperature and diluted with water (5 mL). The solid obtained was filtered at pump and washed with water:ethanol (2:1). The product was recrystallized with ethanol. The products were characterized by their spectral data.

While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 538-58-9.

Reference£º
Article; Aggarwal, Komal; Khurana, Jitender M.; Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy; vol. 143; (2015); p. 288 – 297;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate

A common heterocyclic compound, 4254-15-3,(S)-Propane-1,2-diol, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route. 4254-15-3

Example 29; N-r(2Z)-3-butviri.31thiazolor4.5-clpyridin-2(3H)-ylidenel-2-(r(2S)-2-hvdroxypropylloxyl-5 -(trifluoromethyl)benzamide; (S)-propane-l,2-diol (52 mg, 0.68 mmol) in THF (1 mL) was treated with NaH (60percent dispersion; 27 mg, 0.68 mmol) at room temperature for 20 minutes. The mixture was cooled to O0C and a solution of Example 2OB (90 mg, 0.23 mmol) in THF (1 mL) was added. The mixture was allowed to warm to room temperature, and stirred for 4 hours. The mixture was diluted with saturated aqueous NaHCO3 (20 mL) and extracted with ethyl acetate (2 x 30 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered, and concentrated. The residue was purified by column chromatography using an Analogix.(R). Intellifiash280 .(TM). (SiO2, 0-100 percent ethyl acetate in hexanes) to afford 19 mg (19percent) of the title compound. 1H NMR (500 MHz, CDCl3) delta ppm 1.04 (t, J=7.48 Hz, 3 H) 1.28 (d, J=6.41 Hz, 3 H) 1.47 – 1.59 (m, 2 H) 1.88 – 1.98 (m, 2 H) 3.87 (t, J=8.85 Hz, 1 H) 4.21 – 4.31 (m, 1 H) 4.35 (dd, J=9.15, 2.75 Hz, 1 H) 4.51 – 4.59 (m, 2 H) 7.12 (d, J=8.85 Hz, 1 H) 7.72 (dd, J=8.54, 2.14 Hz, 2 H) 8.51 (d, J=I.83 Hz, 2 H) 8.75 (s, 1 H); MS (DCI/NH3) m/z 454 (M+H)+., 4254-15-3

This compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route,(S)-Propane-1,2-diol,4254-15-3,its application will become more common.

Reference£º
Patent; ABBOTT LABORATORIES; FROST, Jennifer, M.; LATSHAW, Steven, P.; DART, Michael, J.; CARROLL, William, A.; PEREZ-MEDRANO, Arturo; KOLASA, Teodozyj; PATEL, Meena; NELSON, Derek, W.; LI, Tongmei; PEDDI, Sridhar; WANG, Xueqing; LUI, Bo; WO2010/71783; (2010); A1;,
Synthesis and Crystal Structure of a Chiral?C3-Symmetric Oxygen Tripodal Ligand and Its Applications to Asymmetric Catalysis
Chiral lanthanide(III) complexes of sulphur¨Cnitrogen¨Coxygen ligand derived from aminothiourea and sodium?D-camphor-¦Â-sulfonate