Month: August 2021

Electric Literature of 42726-73-8,Some common heterocyclic compound, 42726-73-8, name is tert-Butyl methyl malonate, molecular formula is C8H14O4, 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.

To a mixture of tert-butyl methyl malonate (31.1 g, 179 mmol) and magnesium chloride(17.02 g, 179 mmol) in 350 mL acetonitrile at 0°C is added triethylamine (100 mL, 715mmol). The mixture is stirred for 15 minutes at 0°C. 3-(benzyloxy)-4-oxo-4H-pyran-2-carbonyl chloride (43 g, 162 mmol) in acetonitrile (30 mL) is added dropwise. The reaction mixture is allowed to warm to room temperature and stirred for two hours. The reaction mixture is cooled to 0°C and quenched with 30 mL 6N HCI. To the resulting mixture is added 1 L ether and the mixture is transferred to a separatory funnel. The aqueous layer is removed and the organics are washed with 2 X 300 mL water followed by washings with brine until the ether layer is clear. The organic layer is dried over magnesium sulphate, filtered, then concentrated to give 1-(tert-butyl) 3-methyl 2-(3-(benzyloxy)-4-oxo- 4H-pyran-2-carbonyl)malonate which is used without further purification.

The synthetic route of 42726-73-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; NOVARTIS AG; JAIN, Rama; KOESTER, Dennis Christofer; MANNING, James R.; SUTTON, James Clifford; TAFT, Benjamin R.; WAN, Lifeng; ZHAO, Qian; (148 pag.)WO2017/153919; (2017); A1;,
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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. 53518-15-3, name is 7-Amino-4-(trifluoromethyl)-2H-chromen-2-one, A new synthetic method of this compound is introduced below., Formula: C10H6F3NO2

In a 25 mL reaction tube, add coumarin 151 (45.8 mg, 0.2 mmol), sodium bromide (30.8 mg, 0.3 mmol), sodium bisulfate hydrate (55.2 mg, 0.4 mmol), water (72 mg, 4 mmol) And acetonitrile (2mL), stirred under the irradiation of three 2-watt LED lamps for 17 hours, after the reaction was completed, extracted, dried, filtered, concentrated, and separated by column chromatography to obtain a yellow solid 2q (48mg, 81%);

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; East China Normal University; Jiang Xuefeng; Lu Lingling; Li Yiming; (19 pag.)CN111138307; (2020); A;,
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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. 426-65-3, name is Ethyl Pentafluoropropionate, A new synthetic method of this compound is introduced below., Computed Properties of C5H5F5O2

Sodium ethoxide (7.49 g, 0.11 mol) was suspended in methyl tert-butyl ether (anhydrous, 200ml) under nitrogen. Ethyl 2,2,3, 3,3-pentafluoropropanoate (14.8 ml, 0.1 mol) was added dropwise with stirring followed by ethyl acetate (10.7 ml, 0.11 mol). Stirring was continued for 45 minutes at ambient temparature, for one hour at 50C and overnight at ambient tempeature. The mixture was cooled to 0C and acidified with HC1 (1M, 80 ml), brine was added (80 ml), the layers were separated, and the aqueous layer was back-extracted with in methyl tert-butyl ether (80 ml). The combined organic layers were dried over Na2S04and concentrated under reduced pressure to yield 14.6 gram (0.062 mol, 62% yield). H-NMR (300 MHz, CDC13): delta 1 1.96 (s), 5.59 (s), 4.11-4.26 (m), 3.70 (m), 1.21-1.29 (m);19F-NMR (282 MHz, CDC13): delta -81.8 (s), -83.3 (s), -122.7 (s), -123.6 (s); MS 189 (M-OCH2CH3)

The synthetic route of 426-65-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; INTERVET INTERNATIONAL B.V.; INTERVET INC.; BERGER, Michael; VEIT, Stephan; NIEDERMANN, Hans, Peter; KAPPESSER, Tobias; STUTZ, Alfred; WO2015/177179; (2015); A1;,
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Application of 26759-46-6, The chemical industry reduces the impact on the environment during synthesis 26759-46-6, name is Methyl 2-amino-4,5-dimethoxybenzoate, I believe this compound will play a more active role in future production and life.

General procedure: A mixture of 2-aminobenzoic acid (0.1 mol) and formamide (20 mL)was refluxed for 10 h. After the mixture was cooled to room temperature,water (200 mL) was added and the precipitate was filtered off. Thecrude product was recrystallized from ethanol (100 mL) to the desiredintermediate 1 as a white solid.

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, Methyl 2-amino-4,5-dimethoxybenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Xie, Dandan; Shi, Jing; Zhang, Awei; Lei, Zhiwei; Zu, Guangcheng; Fu, Yun; Gan, Xiuhai; Yin, Limin; Song, Baoan; Hu, Deyu; Bioorganic Chemistry; vol. 80; (2018); p. 433 – 443;,
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Related Products of 91367-05-4,Some common heterocyclic compound, 91367-05-4, name is Methyl 4-chloro-3-methylbenzoate, molecular formula is C9H9ClO2, 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.

Preparation 2Methyl 3 -bromomethyl-4-chlorobenzoate Into an appropriate flask methyl 4-chloro-3-methylbenzoate (25.26 g), N- bromosuccinimide (24.85 g) and 20 ml of carbon tetrachloride were placed. The reaction mixture was refluxed for about 6 hours. After cooling to 25 0C, 500 ml dichloromethane and 300 ml of aqueous solution Of K2CO3 (5 %) were added. The separated aqueous layer was extracted again with 200 ml of dichloromethane. The combined organic layers were washed with 300 ml of aqueous solution of K2CO3 (5 %), dried over Na2SO4 and concentrated in vacuum to give 35.66 g of pale yellow crystals. Distillation under reduced pressure allowed to separate 6.72 g of the starting methyl 4-chloro-3-methylbenzoate (b.p. 80-100 0C / 0.44-0.40 mbar) and to obtain 25.53 g of the desired product as pale yellow crystals (b.p.110 0C /0.40 mbar, m.p. 93 0C). Yield: 71 % (distilled product) T.L.C.: Silica gel, eluents: cyclohexane-ethyl acetate 85/15

The synthetic route of 91367-05-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI-AVENTIS; WO2006/79857; (2006); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 773873-90-8, name is Methyl 5-fluoro-2-(trifluoromethyl)benzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. name: Methyl 5-fluoro-2-(trifluoromethyl)benzoate

Example 15a) 5-Dimethylamino-2-trifluoromethyl-benzoic acid methyl ester (15a)To a stirred solution of 4,48 g (22.5 mmol) 5-Fluoro-2-trifluoromethyl-benzoic acid methyl ester (Rarechem) and 60.0 ml dimethylsulphoxid were added 2.23 g (27.0 mmol) dimethylamine hydrochloride and 6.54 g (47.3 mmol) potassium carbonate. The reaction mixture was stirred for 8h at 600C in an autoclave and was reduced with high vacuum rotation evaporator at 650C. The residue was diluted with dichloromethane, washed twice with water. The combined water phases were extracted with dichloromethane. The combined dichloromethane phases were washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude was purified by column chromatography and the desired product 15a was obtained in 72 % yield (4,00 g, 16,2 mmol).MS-ESI: 248 (M+ +1 , 100). Elementary analysis: C 53.44% H 4.89% F 23.05% N 5.67% Determined: C 53.45% H 4.90% F 23,05% N 5.65%

The synthetic route of 773873-90-8 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BAYER SCHERING PHARMA AKTIENGESELLSCHAFT; WO2008/28688; (2008); A2;,
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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. 76308-28-6, name is Ethyl 2-(trans-4-aminocyclohexyl)acetate, A new synthetic method of this compound is introduced below., Recommanded Product: 76308-28-6

Take 5.0 g (0.032 mol) of the compound ethyl 2- (4-aminocyclohexyl) acetate,Add 50ml of dichloromethane, 8.5g (2eq) of 30% sodium hydroxide solution,Added under stirring N, N- dimethylformamide chloride 6.9g (0.064mol),The reaction was stirred at 30 C for 5h.Point the plate to control, and the reaction is over. Add 50ml of water to the reaction system.Stir for 5 minutes and separate the layers, separate the organic phase, dry and spin dry to obtain 5.2 g of the compound of formula I;

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Shangyu Jing Xin Pharmaceutical Co., Ltd.; Zhejiang Jingxin Pharmaceutical Co., Ltd.; Shanghai Jingxin Bio-pharmaceutical Co., Ltd.; Zhang Min; Zheng Fei; (11 pag.)CN110317182; (2019); A;,
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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. 14064-10-9, name is Diethyl 2-chloromalonate, A new synthetic method of this compound is introduced below., COA of Formula: C7H11ClO4

EXAMPLE 1 195 g of diethyl chloromalonate were dissolved in 500 ml of acetonitrile, and 320 g of the addition product of 3 mol of hydrogen fluoride and 1 mol of triethylamine were added in the absence of moisture. 100 g of triethylamine were then added and the mixture was stirred at an internal temperature of 80° C. until conversion was complete. The solvent was then distilled off and the residue was poured into water. The diethyl fluoromalonate of formula (Ia) obtained was extracted with methylene chloride and the extract was washed with saturated aqueous sodium hydrogencarbonate solution, dried over magnesium sulphate and fractionated under high vacuum. The yield was 147 g=83percent of theory.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Bayer Aktiengesellschaft; US5391811; (1995); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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 35598-05-1 as follows. Safety of Methyl 4-methoxy-2-methylbenzoate

To a solution of methyl 4-methoxy-2-methylbenzoate (11.4 g, 63.3 mmol) in THF (65 mL) at 0 C, LiAlH4 (1M in ether, 76.0 mL, 75.9 mmol) was added via addition funnel over 50 min. The ice water bath was removed, and the reaction was allowed to stir at room temperature for 30 min. Upon completion, the reaction was cooled to 0 C and sodium sulfate decahydrate was added portionwise until the bubbling ceased. The reaction was then diluted with ether and filtered. The filtrate was concentrated under reduced pressure to give (4-methoxy-2- methylphenyl)methanol (8.2 g) as a clear oil. ¾ NMR (300MHz, CDC13): delta 7.23 (d, 1H), 6.72 (m, 2H), 4.63 (d, 2H), 3.79 (s, 3H), 2.36 (s, 3H), 1.42 (t, 1H).

According to the analysis of related databases, 35598-05-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ARAGON PHARMACEUTICALS, INC.; KAHRAMAN, Mehmet; GOVEK, Steven, P.; NAGASAWA, Johnny, Y.; SMITH, Nicholas, D.; WO2011/156518; (2011); A2;,
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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. 57486-67-6, name is Methyl 2-(2-fluorophenyl)acetate, A new synthetic method of this compound is introduced below., Recommanded Product: Methyl 2-(2-fluorophenyl)acetate

Example 15: Synthesis of 3-(2-Chloro-phenyl)-6-(2-fluoro-benzyi)-lH-pyrazolo[3,4-b]- pyrazine; Step 1. Preparation of [6-Chloro-5-( 2-chloro-benzoyl)-pyrazin-2-yl]-( 2-fluoro-phenyl)- acetic add methyl ester; To a solution of sodium hydride (0.175 g, 7 mmol) and (2-Chloro-phenyl)-(3,5-dichloro- pyrazin-2-yl)-methanone (0.86 g, 2.99 mmol) in 5 mL DMF was added (2-Fluoro-phenyl)- acetic acid methyl ester (0.503 g, 2.99 mmol). The reaction mixture was stirred for one hour at RT, and then was quenched by addition of water and aqueous HCl. The aqueous mixture was extracted with methylene chloride, and the combined organic phases were dried over MgSO4, filtered, and evaporated under reduced pressure to give 1.19 g of crude [6-Chloro-5-(2-chloro-benzoyl)-pyrazin-2-yl]-(2-fluoro-phenyl)-acetic acid methyl ester. Mass Spec. M+H = 419.

The synthetic route of 57486-67-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; WO2007/23105; (2007); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics