Author: tianli

With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.81335-87-7, name is (2-Amino-4-methylphenyl)methanol, molecular formula is C8H11NO, molecular weight is 137.18, as common compound, the synthetic route is as follows.Safety of (2-Amino-4-methylphenyl)methanol

To a solution of (2-amino-4-methylphenyl)-methanol (3.2 g, 23.4 mmol) in THF (40 mL) is added di-ferf-butyl dicarbonate (6.54 g, 28.0 mmol) and the solution is stirred at 60 0C for 5 h. The solvent is evaporated, and water is added. It is then extracted with EtOAc, washed with water, dried with MgSO4 and concentrated. The residue is purified to give the title compound.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,81335-87-7, (2-Amino-4-methylphenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; NOVARTIS AG; NOVARTIS PHARMA GmbH; WO2007/67612; (2007); A1;,
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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 compound 13651-14-4, name is (2,3-Dimethylphenyl)methanol. This compound has unique chemical properties. The synthetic route is as follows. SDS of cas: 13651-14-4

To a dichloromethane solution (0.2 M) of (2,3-dimethylphenyl)methanol (1 eq.) from the previous step was added triethylamine (1.2 eq.) and then methanesulfonyl chloride (1.1 eq.) at 0 0C. The reaction mixture was stirred at 0 0C for 20 min before it was quenched with sat. aq. NaHCO3. The aqueous layer was separated and back-extracted with dichloromethane. The combined organic extracts were then dried over Na2SO4, filtered and the filtrate concentrated in vacuo to furnish the title compound as a colorless oil.

With the rapid development of chemical substances, we look forward to future research findings about 13651-14-4.

Reference:
Patent; MERCK FROSST CANADA LTD.; CHIH-YU CHEN, Austin; LALIBERTE, Sebastien; LAROUCHE, Guillaume; HAN, Yongxin; MCKAY, Daniel; WO2011/20193; (2011); A1;,
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Application of 813-99-0 ,Some common heterocyclic compound, 813-99-0, molecular formula is C5H9Cl3O, 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.

EXAMPLE 46; Preparation of 8-[4-(Difluoromethoxy)phenyl]-8-[3-(2-fluoropyridin-3-yl)phenyl]-2,8-dihydrospiro[imidazo[1,5-a]pyrimidine-3,3′-oxetan]-6-amine; Step a) Preparation of Compound 2; A mixture of 1 (1.0 g, 5.22 mmol) and potassium hydroxide (0.345 g of 85%, 5.22 mmol) in ethanol (2 mL) was heated at reflux for 3 h. The reaction was cooled to room temperature, diluted with ethyl acetate (10 mL) and the solids that formed removed by filtration. The filtrate was concentrated to afford 2 (0.65 g, 80%) as a colorless liquid: 1H NMR (300 MHz, CDCl3) delta 4.47 (s, 4H), 3.95 (s, 4H).

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. 813-99-0, 3-Chloro-2,2-bis(chloromethyl)propan-1-ol, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Wyeth; US2005/282826; (2005); A1;,
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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. 15100-35-3, name is Bicyclo[4.2.0]octa-1,3,5-trien-7-ylmethanol, the common compound, a new synthetic route is introduced below. COA of Formula: C9H10O

Step B. p-Toluenesulfonyl chloride (662 mg, 3.47 mmol), triethylamine (0.605 ml), and DMAP (35 mg, 0.29 mmol) were added to a solution of bicyclo[4.2.0]octa-1,3,5-trien-7-ylmethanol (388 mg, 2.89 mmol) in dichloromethane (12 mL) at room temperature and the reaction mixture was stirred overnight. Saturated aqueous NH4CI was added to the reaction mixture, and the mixture was extracted with dichloromethane, dried over MgSO4 and purified by chromatography (5-20% EtOAc/hexanes) to provide bicyclo[4.2.0]octa-1,3,5-trien-7-ylmethyl 4-methylbenzenesulfonate (830 mg, 99%).

The synthetic route of 15100-35-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KNOPP BIOSCIENCES LLC; Resnick, Lynn; Topalov, George T.; Boyd, Steven A.; Belardi, Justin K.; Flentge, Charles A.; Hale, James S.; Harried, Scott S.; Mareska, David A.; Zhang, Kai; Heap, Charles R.; Hadden, Mark; Cui, Wenge; Decornez, Helene; Liu, Shuang; (146 pag.)US2016/31875; (2016); A1;,
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Reference of 55357-38-5, Adding some certain compound to certain chemical reactions, such as: 55357-38-5, name is 2-Hydroxy-N,N,N-trimethylethanaminium 4-methylbenzenesulfonate,molecular formula is C12H21NO4S, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 55357-38-5.

P1-(cytidin-5′-yl)-P2-(trimethylammoniumethyl)-methylenebis(phosphonate) is an analog of cytidyl diphosphocholine (citicholine), an important intermediate in lipid metabolism and a drug under development for treatment for ischemic stroke. The analog may be prepared by the reaction of the appropriate BTA with a p-toluenosulfonate salt of choline. Thus, a mixture of the BTA prepared from N4-acetylcytidin-5′-ylphosphonomethylenephosphonic acid (1 mmol in 10 ml of dry pyridine) and p-toluenosulfonate salt of choline (412 mg, 1.5 mmol) is kept at 55C for 4 hours. The mixture is processed as described in Example 3. P1-(N4-acetyl-2′,3′-O-isopropylidenecytidin-5′-yl)-P2-(trimethylammoniumethyl)-methylenebisphosphonate is obtained, and deprotected with Dowex 50WX8/H+ to give the desired compound.

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. 55357-38-5, 2-Hydroxy-N,N,N-trimethylethanaminium 4-methylbenzenesulfonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Pharmasset, Ltd.; EP1469003; (2004); A2;,
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Adding a certain compound to certain chemical reactions, such as: 54410-90-1, 4-Pentylcyclohexanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Computed Properties of C11H22O, blongs to alcohols-buliding-blocks compound. Computed Properties of C11H22O

Step 2:2L four bottles of the first step to add 200.8g (1179.0mmol, 1.0eq), 800.0 g of dichloroethane, 131.2 g (1279.0 mmol, 1.1 eq) of triethylamine, 14.4 g (117.8 mmol, 0.1 eq) of 4-dimethylaminopyridine,Into the ice machine cooling to -5 ~ 0 stand.A solution of 148.6 g (1297.0 mmol, 1.1 eq) of methanesulfonyl chloride and 200.8 g of dichloroethane was added dropwise over 1.5 h, and the dropping temperature was controlled at -5 to 5 C,Followed by 0 ~ 5 insulation stirring 1.0h.Add water 600g quenching reaction, then stop the cooling, the kettle temperature to room temperature, stirring 0.5h, standing for 0.5h, divided into an oil layer 1268.0g, the water back to the kettle by adding dichloroethane 200.0g secondary extraction, stirring 0.5 h, standing for 0.5h, separate the secondary reservoir 188.7g.Combined with a secondary oil layer, add water 400.0g washing, stirring 0.5h, standing for 0.5h, separated from the oil layer, desolvation, the use of ethanol to get 260.0g two-step product, the content of> 98%, yield 88% Cis – trans isomer ratio 56/44.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,54410-90-1, 4-Pentylcyclohexanol, and friends who are interested can also refer to it.

Reference:
Patent; Dalian Jiu Xin Fine Chemical Co., Ltd.; Dai Yao; Liang Quande; Zhao Danyang; Liu Lingling; Wang Weixin; Wang Rongliang; (5 pag.)CN106916089; (2017); A;,
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Adding a certain compound to certain chemical reactions, such as: 55357-38-5, 2-Hydroxy-N,N,N-trimethylethanaminium 4-methylbenzenesulfonate, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, Formula: C12H21NO4S, blongs to alcohols-buliding-blocks compound. Formula: C12H21NO4S

(R) -1,2-glyceryl distearate-glycerol-3-phosphatidic acid (0.2 g, 0.28 mmol)Was added to 60 mL of dry pyridine,It was heated at 50 0.5h,Then, choline p-toluenesulfonate (0.84 g, 3 mmol)And trichloroacetonitrile 5mL,The reaction was continued at 50 36h,Concentration under reduced pressure crude,Flash column chromatography (developing solvent CHCl3-CH3OH-H2O, 15: 5: 1) gave a white gel, 0.13 g, 59% yield.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,55357-38-5, 2-Hydroxy-N,N,N-trimethylethanaminium 4-methylbenzenesulfonate, and friends who are interested can also refer to it.

Reference:
Patent; Ji, Min; Cai, Jin; Gu, Ning; Li, Rui; (7 pag.)CN103408588; (2016); B;,
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Adding a certain compound to certain chemical reactions, such as: 626-95-9, 1,4-Pentanediol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, SDS of cas: 626-95-9, blongs to alcohols-buliding-blocks compound. SDS of cas: 626-95-9

General procedure: An aqueous solution containing 1,4-butanediol (0.5 mmol),cyclohexene (5 mmol, 0.506 mL, 10 equiv), KOH (25 mol%,0.007 g, 0.125 mmol), and 1 or 2 (10 mol%, 0.0506 g or 0.051 g,0.05 mmol) was heated to 100 C for 48 h in a sealed vessel. Oncompletion of the reaction, the products were extracted withDCM and injected into gas chromatography. gamma-Butyrolactonewith 73% and 84% yields was observed with the formation ofcyclohexane with 22% and 24% yields.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,626-95-9, 1,4-Pentanediol, and friends who are interested can also refer to it.

Reference:
Article; Bhatia, Anita; Kannan, Muthukumar; Muthaiah, Senthilkumar; Synlett; vol. 30; 6; (2019); p. 721 – 725;,
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Adding a certain compound to certain chemical reactions, such as: 261763-21-7, (5-Chloro-2-(trifluoromethyl)phenyl)methanol, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, COA of Formula: C8H6ClF3O, blongs to alcohols-buliding-blocks compound. COA of Formula: C8H6ClF3O

To a solution of(5-chloro-2- (trifluoromethyl)phenyl)methanol (400 mg, 1.90 mmol)and triethylamine (0.794 mL, 5.70mmol) in DCM (8 mL) was added methanesulfonyl chloride (0.148 mL, 1.90 mmol) at 0C. The reaction was stirred for 1 hour at 0 C, then quenched with water (10 mL) and extracted with DCM (10 mL x 3). The combined organic layers were washed with brine (saturated, 10 mL), dried over Mg504 and filtered. The filtrate was concentrated under reduced pressure to give the title compound, which was used in the next step without purification.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,261763-21-7, (5-Chloro-2-(trifluoromethyl)phenyl)methanol, and friends who are interested can also refer to it.

Reference:
Patent; MERCK SHARP & DOHME CORP.; MILLER, Michael; CHOBANIAN, Harry, R.; HE, Shuwen; HAO, Jinsong; PIO, Barbara; GUO, Yan; XIAO, Dong; (213 pag.)WO2018/118670; (2018); A1;,
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Adding a certain compound to certain chemical reactions, such as: 55977-10-1, 3-Bromo-7-hydroxy-4-methylchromen-2-one, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound, category: alcohols-buliding-blocks, blongs to alcohols-buliding-blocks compound. category: alcohols-buliding-blocks

General procedure: The appropriate 7-hydroxycoumarin 1a-g (2.0 mmol for 2a-gand 2i-r; 3.0 mmol for 1h) was suspended in anhydrous acetone(10 mL) before adding potassium carbonate (for 2a-g and 2i-r: 0.83 g, 6.0 mmol; for 1h: 1.2 g, 9.0 mmol), the suitable monohalide(for 1h: 2-[4-(bromomethyl)phenyl]ethanol, 3.0 mmol) or dihalide(for 2a-g and 2i-r: 6.0 mmol of alpha,alpha’-dibromo(chloro)-xylenes or trans-1,4-dibromo-2-butene; 10 mmol of 1,omega-dibromoalkanes) anda catalytic amount of KI in a Pyrex vessel charged with a magnetic stirring bar and aWeflon bar. The vessel was placed in a microwave apparatus and irradiated at 130 C for 30 min. After cooling to room temperature, the inorganic residue was filtered off after thorough washing with CH2Cl2. The solutionwas concentrated to dryness andthe resulting crude was purified as detailed below.

At the same time, in my other blogs, there are other synthetic methods of this type of compound,55977-10-1, 3-Bromo-7-hydroxy-4-methylchromen-2-one, and friends who are interested can also refer to it.

Reference:
Article; Rullo, Mariagrazia; Niso, Mauro; Pisani, Leonardo; Carrieri, Antonio; Colabufo, Nicola Antonio; Cellamare, Saverio; Altomare, Cosimo Damiano; European Journal of Medicinal Chemistry; vol. 161; (2019); p. 433 – 444;,
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