Esters-buliding-blocks

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. 369-25-5, name is Methyl 3,4-difluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. COA of Formula: C8H6F2O2

a) 3-Fluoro-4-dimethylamino-benzoic acid methyl ester (3a) To a stirred solution of 38,7g (225 mmol) 3.4-difluoro-benzoic acid methyl ester (Apollo) and 600 ml dimethylsulphoxid are added 22.3 g (270 mmol) dimethylamine hydrochloride and 65.4 g (473 mmol) potassium carbonate. The reaction mixture is stirred for 5h at 55C in an autoclave and is reduced with high vacuum rotation evaporator at 65C. The residue is diluted with dichloromethane, washed twice with water. The combined water phases are extracted with dichloromethane. The combined dichloromethane phases are washed with diluted sodium hydrogen carbonate solution, dried with sodium sulphate and concentrated. The oily crude product 3a is obtained in 71% yield (31.5 g, 160.0 mmol) and is used for the next step without purification. MS-ESI: 198 (M+ +1, 72).

The synthetic route of 369-25-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Bayer Schering Pharma Aktiengesellschaft; EP1897885; (2008); A1;,
Ester – Wikipedia,
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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. 28868-76-0, name is Dimethyl 2-chloromalonate, A new synthetic method of this compound is introduced below., Quality Control of Dimethyl 2-chloromalonate

(1) In a 1 L reaction flask equipped with mechanical stirring, temperature display and distillation column, 430 ml of anhydrous dioxane was added.166.6 g of dimethyl chloromalonate and 10 g of dried potassium iodide;(2) 87.5 g of anhydrous potassium fluoride was activated by microwave drying, and added to the above reaction bottle;(3) heating to 100 C under reflux, and reacting for 1 hour;(4) collecting a fraction of 74-78 C through a distillation column;(5) The distillation temperature is up to 78 C to stop heating, to obtain crude dimethyl 2-fluoromalonate;(6) A total of 160g of crude product was collected, and the content of dimethyl 2-fluoromalonate was 91.6%, which was equivalent to 146.6 g of pure product;(7) Refining obtained 136 g of dimethyl 2-fluoromalonate, the content was 99.5%, and the yield was 90.2%.

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; Sinopharm Group Chemical Reagent Co., Ltd.; Guo Jianguo; Gu Xiaoyan; Wu Xiaolan; Huang Hao; (4 pag.)CN109824512; (2019); A;,
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Some common heterocyclic compound, 935273-86-2, name is Benzyl 3,3-difluorocyclobutanecarboxylate, molecular formula is C12H12F2O2, 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. category: esters-buliding-blocks

Benzyl 3,3-difluorocyclobutanecarboxylate (2-C) (0.84 g, 3.72 mmol) was dissolved in ethanol (40 ml), and approximately 20 mg of palladium on activated carbon was added. The mixture was stirred at room temperature under hydrogen atmosphere for 12 hours, and then filtered through a pad of Celite. The filtrates were concentrated and dried in vacuo to give 2-D. lH NMR (500 MHz, CDCI3): delta2.86-2.93 (4H, m), 3.02-3.04 (IH, m) ppm.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 935273-86-2, its application will become more common.

Reference:
Patent; MERCK & CO., INC.; WO2007/47625; (2007); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 403-33-8, name is Methyl 4-fluorobenzoate, A new synthetic method of this compound is introduced below., Quality Control of Methyl 4-fluorobenzoate

General procedure: Carboxylic acid hydrazides are synthesized following a modifiedprocedure from one already reported in the literature [22]. Hydrazinehydrate (80%, 0.06 mol) is added slowly to a solution ofcarboxylate esters (0.02 mol) in methanol (30 mL). The reactionmixture is subjected to reflux for 6-8 h. Upon completion of reaction,the mixture is cooled down to the room temperature and icewater is added. The precipitated solid product obtained wasfiltered, dried and recrystallized from methanol.

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:
Article; Hamdani, Syeda Shamila; Khan, Bilal Ahmad; Ahmed, Muhammad Naeem; Hameed, Shahid; Akhter, Kulsoom; Ayub, Khurshid; Mahmood, Tariq; Journal of Molecular Structure; vol. 1200; (2020);,
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Application of 99548-54-6, A common heterocyclic compound, 99548-54-6, name is Methyl 3-bromo-2-methylbenzoate, molecular formula is C9H9BrO2, 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.

Compound I-1B (4.56 g, 20 mmol) was dissolved in anhydrous THF (100 mL).After cooling to 0 C, LAH (0.8 g, 20 mmol) was added in portions to maintain the internal temperature of the reaction solution less than 5 C. After the addition, the temperature was slowly raised to room temperature for 2 hours.TLC showed that after the reaction was over, it was re-cooled to 0 C, 0.8 ml of water was added dropwise, 0.8 ml of 15% NaOH and 2.4 ml of water were added, and after stirring, the mixture was stirred for 1 hour and filtered.The obtained filtrate was dried to give Compound I-1C (3.7 g, yellow solid).Yield: 92.4%.

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; Guangzhou Dankang Pharmaceutical Biological Co., Ltd.; Xu Yong; Huang Lu; Lin Dang; Hu Hai; (29 pag.)CN110092740; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 6279-86-3, 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. 6279-86-3, name is Triethyl methanetricarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Example IEthyl 2,4-dihvdroxy-7,7-dimethyl-5-oxo-5,6,7,8-tetrahvdroquinoline-3-carboxylate10 g 3-Amino-5,5-dimethyl-2-cyclohexen-1-one and 25 g 2-Ethoxycarbonyl-malonic acid diethyl ester are combined and heated for 10 minutes at 210C (bath temperature).Thereafter the mixture is cooled to room temperature and triturated with diethylether. The crystalline precipitate is collected by filtration and dried in vacuo.Yield: 9,9 g (49 % of theory)Mass spectrometry (ESI+): m/z = 280 [M+H]+ Rf-value: 0,45 (silica gel, dichloromethane/methanol 9: 1)

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, Triethyl methanetricarboxylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; WAGNER, Holger; BERTA, Daniela; FUCHS, Klaus; GIOVANNINI, Riccardo; HAMPRECHT, Wolfgang; KONETZKI, Ingo; STREICHER, Ruediger; TRIESELMANN, Thomas; WO2012/110599; (2012); A1;,
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Application of 34837-84-8,Some common heterocyclic compound, 34837-84-8, name is Methyl 2-(4-fluorophenyl)acetate, molecular formula is C9H9FO2, 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.

Stir at 0 C,To sodium hydride (60% in mineral oil, 2.62 g, 65.5 mmol)Anhydrous tetrahydrofuran (60 mL)Methyl 2-(4-fluorophenyl)acetate (IV-1, 5 g, 29.73 mmol) was added dropwise to the suspension.The resulting mixture was stirred at 0 C for 0.5 hours.Then slowly add methyl iodide (12.7 g, 89.4 mmol).After the addition was completed, the reaction mixture was stirred at 50 C for 5 hours.Quenched with ice water (100 mL),Extracted with ethyl acetate (40 mL ¡Á 3).Combine the organic phase,Dried over anhydrous sodium sulfate,Filter and concentrate in vacuo,Made yellow oilMethyl 2-(4-fluorophenyl)-2-methylpropanoate(IV-2, 5.7 g, yield: 98%).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 2-(4-fluorophenyl)acetate, its application will become more common.

Reference:
Patent; Guangzhou Yingsheng Biological Technology Co., Ltd.; Li Jingrong; Li Anhu; (57 pag.)CN110092804; (2019); A;,
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Ester – an overview | ScienceDirect Topics

Related Products of 24807-40-7, 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. 24807-40-7 name is Methyl 3-(4-(benzyloxy)phenyl)propanoate, 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.

2 N Sodium hydroxide aqueous solution (3.5 mL) and water (10 mL) were added to a tetrahydrofuran-methanol solution (20 mL-10 mL) of the compound obtained in (1) (1.60 g), and stirred for 1 hour at 60C. The reaction solution was made acidic with 1 N hydrochloric acid, and then extracted with diethyl ether. The extract was washed with saturated sodium chloride solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was recrystallized from diethyl ether-hexane to obtain 3-[4-(benzyloxy)phenyl] propionic acid (1.27 g) as colorless crystals. 1H-NMR (300MHz, CDCl3); delta 2.65 (2H, t, J=7.8Hz), 2.91 (2H, t, J=7.8Hz), 5.04 (2H, s), 6.91 (2H, d, J=8.7Hz), 7.13 (2H, d, J=8.7Hz), 7.29-7.45 (5H., m)

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 3-(4-(benzyloxy)phenyl)propanoate, and friends who are interested can also refer to it.

Reference:
Patent; Takeda Pharmaceutical Company Limited; EP1849465; (2007); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 23877-12-5, These common heterocyclic compound, 23877-12-5, name is tert-Butyl 2-bromo-2-methylpropanoate, 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.

Production Example 10 Synthesis of tert-Butyl 2-[2-[2-[N-2-(4-chlorophenoxy)ethylaminocarbonyl]ethyl]phenoxy]-2-methylpropionate N-(4-Chlorophenoxyethyl)-3-(2-hydroxyphenyl)propanamide (11.6 g, 36.3 mmol) was dissolved in acetonitrile (15 mL), and potassium carbonate (15.0 g, 109 mmol) was added thereto. Subsequently, tert-butyl 2-bromoisobutyrate (20.2 g, 90.7 mmol) was added thereto, followed by stirring for 4 days at 70 C. Subsequently, water was added thereto, and the resultant mixture was extracted with ethyl acetate. The organic layer was washed with brine, and the resultant mixture was subjected to drying over anhydrous sodium sulfate, concentration under reduced pressure, and purification by silica gel chromatography (chloroform/methanol=50/1), whereby the target compound was obtained (7.4 g, 44%).

The synthetic route of 23877-12-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; KOWA CO., LTD.; US2005/101636; (2005); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 105-53-3, 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 105-53-3 as follows.

Synthesis of 2-ethoxycarbonyl-malonic acid diethyl ester; Magnesium turnings (1.25 g, 50.2 mmol), dry ethanol (5 ml.) and CCI4 (0.5 ml_) were taken in a dry 100 mL of three neck flask and it was heated at 80 0C for 6 h. To this was added a mixture of diethyl malonate (8 g, 50.2 mmol) and dry ethanol (14 mL) and stirred for 2 h. The reaction EPO betamixture was cooled in a water bath when crystals were formed. After this, dry THF (20 mL) was added drop wise to dissolve the solid formed and heated for 1 h at 80 0C. To this was then added ethyl chloroformate (5 mL, 50.2 mmol) in dry THF while keeping constant boiling and the heating was further continued for 1 h followed by bringing the reaction mixture to room temperature, poured into dilute acetic acid (4 mL acetic acid in 15 mL water). This was extracted with ethyl acetate, washed with brine and the organic layers were combined and dried over anhydrous Na2SO4 and concentrated to give yellow liquid. The unreacted diethyl malonate was then removed by vacuum distillation to get the pure product as a colorless liquid. 1H NMR (300 MHz, CDCI3): 1.31 (t, 9H), 4.28 (q, 6H), 4.41 (s, 1 H). Mass: 233 (M++1).

According to the analysis of related databases, 105-53-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; INDIAN INSTITUTE OF TECHNOLOGY BOMBAY; WO2006/117800; (2006); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics