Month: June 2021

Reference of 443-26-5, 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. 443-26-5, name is Ethyl 2-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of 2-fluoro-benzoic acid ethyl ester (200 mg; 1.19 mmol; 10 eq.), (1 H-imidazol- 2-ylmethyl)-dimethyl-amine (149 mg; 1.19 mmol; 1 eq.) and cesium carbonate (775 mg; 2.38 mmol; 2 eq.) in DMSO (3 mL) was stirred at 120C for 16 hours. The mixture was diluted with EA, washed with water (3x), dried over magnesium sulfate and concentrated in vacuo to afford the title compound (58 mg, 18%) as a white solid. HPLC (max plot) 95.7%; RM .80 min.

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, Ethyl 2-fluorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK PATENT GMBH; SWINNEN, Dominique; MONTAGNE, Cyril; POMEL, Vincent; QUATTROPANI, Anna; MOLETTE, Jerome; GERBER, Patrick; WO2013/91773; (2013); A1;,
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Synthetic Route of 87-13-8, The chemical industry reduces the impact on the environment during synthesis 87-13-8, name is Diethyl 2-(ethoxymethylene)malonate, I believe this compound will play a more active role in future production and life.

A mixture of aniline (25.6 g, 0.275 mol) and diethyl 2-(ethoxymethylene)malonate (62.4 g, 0.288 mol) was heated at 140-150 C for 2 h. The mixture was cooled to room temperature and dried under reduced pressure to afford 2-phenylaminomethylene-malonic acid diethyl ester as a solid, which was used in the next step without further purification. ‘H NMR (DMSO-rfc) d 11.00 (d, 1H), 8.54 (d, J = 13.6 Hz, 1H), 7.36-7.39 (m, 2H), 7.13-7.17 (m, 3H), 4.17-4.33 (m, 4H), 1.18-1.40 (m, 6H).

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, Diethyl 2-(ethoxymethylene)malonate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; VERTEX PHARMACEUTICALS INCORPORATED; LEE, Elaine Chungmin; NAVAMAL, Mettachit; NTI-ADDAE, Kwame Wiredu; SHI, Yi; SHRESTHA, Muna; ZHANG, Beili; ZWICKER, Carl; (263 pag.)WO2019/191620; (2019); 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. 140-39-6, name is p-Tolyl Acetate, A new synthetic method of this compound is introduced below., HPLC of Formula: C9H10O2

General procedure: A one-necked flask was charged with CuI (10 mg, 0.05 mmol), NaOt-Bu (376 mg, 4.0 mmol), S8 (16 mg, 0.5 mmol), phenolic ester (1 mmol), anhyd DMF (2 mL) under an inert atmosphere. The mixture was magnetically stirred and heated at 120 C for the appropriate reaction time (Table 6). After completion of the reaction, the mixture was cooled to r.t. H2O (4 mL) was added and the product was extracted with EtOAc (3 × 4 mL) and dried (anhyd Na2SO4). Evaporation of the solvent and purification by column chromatography on silica gel (n-hexane/EtOAc) gave the desired symmetrical diaryl sulfides in 75-93% yields.

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; Rostami, Abed; Rostami, Amin; Ghaderi, Arash; Gholinejad, Mohammad; Gheisarzadeh, Sajedeh; Synthesis; vol. 49; 22; (2017); p. 5025 – 5038;,
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Adding a certain compound to certain chemical reactions, such as: 35418-07-6, name is Methyl 3-(4-aminophenyl)propanoate, belongs to esters-buliding-blocks compound, 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 35418-07-6, Formula: C10H13NO2

General procedure: To a solution of 3a (1 g) in ethanol was added Pd/C (5%, 0.1 g) and the mixture was stirred for 24 hrs at room temperature in a hydrogen atmosphere under atmospheric pressure. Insoluble matters were removed using Celite, and the filtrate was concentrated in vacuo to give the desired product 4a (0.76 g) as a yellow solid. To a solution of carboxylic acid (1 equiv) in CH2Cl2 (15 mL) at 0 C was added DMAP (1 equiv) and EDCI (1 equiv). The reaction mixture was stirred at 0 C for 45 minutes. At this time 4a (1 equiv) was added and the mixture was warmed to room temperature and stirred overnight. The resulting mixture was concentrated in vacuo, partitioned between 1.0 M HCl (20 ml) and ethyl acetate (3×20 mL). The combined organic layers were washed with brine (2 × 15 ml), dried over Na2SO4, filtered and concentrated in vacuo. The crude residue was purified by silica gel chromatograph using a mixture of petroleum ether/ethyl acetate (20 : 5, v/v) as eluent to afford the product as a white solid. To a solution of the obtained solid (1 equiv) in 2:3:1 THF/MeOH/H2O (18 ml) was added LiOH·H2O (1.5 equiv). After stirring at room temperature for 4 h, the volatiles were removed under reduced pressure. The residue was acidified with 1N hydrochloric acid solution, and then filtered and the filter cake was washed with 5 mL of water, dried in vacuum to afford a white powder. Recrystallization from 75% EtOH gave the desired compounds 2-17 as 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 3-(4-aminophenyl)propanoate, other downstream synthetic routes, hurry up and to see.

Reference:
Article; Yang, Jianyong; Li, Zheng; Li, Huilan; Liu, Chunxia; Wang, Nasi; Shi, Wei; Liao, Chen; Cai, Xingguang; Huang, Wenlong; Qian, Hai; Bioorganic and Medicinal Chemistry; vol. 25; 8; (2017); p. 2445 – 2450;,
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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. 14062-25-0, name is Ethyl 2-(4-bromophenyl)acetate, A new synthetic method of this compound is introduced below., Formula: C10H11BrO2

A solution of 25g ethyl (4-bromophenyl)acetate in100 ml DMF was added dropwise to 13.8 gpotassium-tert.butylate in 150 ml DMF at 0C and stirred for additional 30 minat 0C. Then 18.4 g bromocyclopentane were added dropwise at 0C and the reactionmixture was stirred until reaction completion. The mixture was given on water,extracted with EE, the combined organic layers washed with water and brine,dried with Na2SO4, filtered and evaporated to dryness.Yield: 35.6 g, used without further purification in the next step.

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; Koppitz, Marcus; Braeuer, Nico; Ter Laak, Antonius; Irlbacher, Horst; Rotgeri, Andrea; Coelho, Anne-Marie; Walter, Daryl; Steinmeyer, Andreas; Zollner, Thomas M.; Peters, Michaele; Nagel, Jens; Bioorganic and Medicinal Chemistry Letters; vol. 29; 18; (2019); p. 2700 – 2705;,
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Some common heterocyclic compound, 4630-80-2, name is Methyl cyclopentanecarboxylate, molecular formula is C7H12O2, 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. Formula: C7H12O2

Example 230 Preparation of 1-(3-Butenyl)cyclopentane Carboxylic Acid Methyl Ester To a solution of diisopropylamine (225 mmol, 31.6 mL) in THF (150 mL) was added dropwise a solution of n-butyl lithium (217.5 mmol, 87 mL, 2.5M) in hexanes at -10 C. while maintaining the temperature below 0 C. After addition, the solution was stirred for 30 min at 0 C. To this, a solution of methyl cyclopentane carboxylate (150 mmol, 19.23 g) in THF (30 mL) was added dropwise at -70 C. maintaining the internal temperature between -60 to -70 C. After addition, the reaction mixture was stirred for 1 h at -50 to -60 C. Then, a solution of 4-bromo-1-butene (142.2 mmol, 19.2 g) in THF (30 mL) was added dropwise and the light brown suspension was stirred for 1 h at -60 to -70 C. Then, it was allowed to warm to room temperature and stirred overnight. The reaction mixture was poured into a saturated solution of ammonium chloride (250 mL) and the mixture was extracted with ether (2*150 mL). The combined extracts were washed with a saturated solution of sodium chloride (150 mL) and dried over anhydrous magnesium sulfate. After filtration of the drying agent, the solution was concentrated under vacuum and the residue was distilled at 63-67 C./2.5 mm Hg to give 13.77 g (53%) of a colorless oil. HR MS (C11H16O2): Obs mass, 182.1311. Calcd mass, 182.1307 (M+).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4630-80-2, its application will become more common.

Reference:
Patent; Hoffmann-La Roche Inc.; US6455550; (2002); B1;,
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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. 125483-57-0, name is Benzyl 1-aminocyclobutanecarboxylate 4-methylbenzenesulfonate, A new synthetic method of this compound is introduced below., category: esters-buliding-blocks

This compound (2.58 g; 0.00686 moles) was reacted with [(2S,3R)-3-benzyloxycarbonylamino-2-hydroxy-4-(4-methylsulfonyl-phenyl)]-butanoic acid (2 g; 0.0049 moles) in a way similar to that described in example 1. A crude (2.9 g) was obtained and crystallized, first, from acetonitrile and, then, from ethanol giving 1[(2S,3R)-3-benzyloxycarbonylamino-2-hydroxy-4-(4-methylsulfonyl-phenyl)-butanoyl]-amino-1-cyclobutanecarboxylic acid benzyl ester (1.74 g; 50% yield) as a white crystalline solid with m.p. 163-165 C. 1 H–NMR (200 MHz, CD3 OD-TMS): delta (ppm): 7.85-7.45 (m, 4H), 7.36-7.18 (m, 10H); nuA =5.15-nuB =5.11 (ABq, JAB =12.4 Hz, 2H); nuA =4.95-nuB =4.88 (ABq, JAB =12.6 Hz, 2H); 4.24 (m, 1H); 3.99 (d,1H, J=2.7 Hz); 3.06 (s, 3H); 3.08-2.84 (m, 2H); 2.68-2.46 (m, 2H); 2.35-2.15 (m, 2H); 2.04-1.84 (m, 2H).

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; Zambon Group, S.p.A.; US5145872; (1992); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2065-23-8, name is Methyl 2-phenoxyacetate, This compound has unique chemical properties. The synthetic route is as follows., Computed Properties of C9H10O3

167.87 g of 99% methyl phenoxyacetate (1 mol) was sequentially added to a 500 mL four-necked flask.1.26 g of 99% zinc chloride and 1.68 g of 99% 4,5-dimethylisothiazole,154.69g of 99% chlorine (2.16 mol) was introduced at -20 C.After the heat preservation reaction for 30 minutes,Distilled at a pressure of 1 kPa and collected at 140-150 CDivided, 236.21g of methyl 2,4-dichlorophenoxyacetate,content98.8%,The yield was 99.28% based on methyl phenoxyacetate.

According to the analysis of related databases, 2065-23-8, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shandong Runbo Biological Technology Co., Ltd.; Sun Guoqing; Hou Yongsheng; Zhang Liguo; Chi Zhilong; Hu Yishan; (12 pag.)CN108947815; (2018); A;,
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Application of 56741-34-5, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 56741-34-5, name is Methyl 5-amino-2-fluorobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: To a solution of compound 11a (154 mg, 1.0 mmol) in anhydrous CH2Cl2 (10 mL) was added 3,5-dichlorobenzoyl chloride (209 mg, 1.0 mmol) and pyridine (241 mL 3.0 mmol) under ice bath. After stirring at room temperature for about 8 h, the solvent was removed in vacuum. The resulting residue was dissolved in NaOH (1 M) water solution (3 mL) and CH3OH (3 mL) and stirred for another 2 h. Then the solvent was removed under vacuum, and the residue was acidied to pH 2 or below with HCl (1 M) water solution. The solution was extracted with ethyl acetate twice and the combined organics were dried over anhydrous sodium sulfate and concentrated in vacuum. The resulting residue was puried by silica gel chromatography to give the desired compound as a white solid (234 mg, yield 85.0%)

The chemical industry reduces the impact on the environment during synthesis Methyl 5-amino-2-fluorobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Article; Gao, Ding-Ding; Dou, Hui-Xia; Su, Hai-Xia; Zhang, Ming-Ming; Wang, Ting; Liu, Qiu-Feng; Cai, Hai-Yan; Ding, Hai-Peng; Yang, Zhuo; Zhu, Wei-Liang; Xu, Ye-Chun; Wang, He-Yao; Li, Ying-Xia; European Journal of Medicinal Chemistry; vol. 154; (2018); p. 44 – 59;,
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Related Products of 5445-17-0, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 5445-17-0, name is Methyl 2-bromopropanoate, This compound has unique chemical properties. The synthetic route is as follows.

Example 7 methyl 2-(2-(pyrrolidin-1-yl)cyclohex-2-en-1-yl)propanoate To a 1 L round bottom flask was added 1-(cyclohex-1-en-1-yl)pyrrolidine (100 g, example 1), acetonitrile (800 mL), methyl 2-bromopropanoate (116.3 g), and sodium iodide (9.9 g). The mixture was then heated to reflux while stirring for 20 hours. The mixture was cooled to room temperature, added DBU (100.3 g), and stirred for 30 minutes. The resulted mixture was then concentrated to remove most acetonitrile, followed by addition of toluene (500 mL). The suspension was stirred at room temperature for 1 hour followed by filtration. The filter cake was washed with small amount of toluene twice. The combined toluene solution was distilled under vacuum to give a liquid product, 143.4 g (91.4%). 1HNMR (CDCl3): delta 4.64 (t, 1H), 3.60 (s, 3H), 2.99 (q, 2H), 2.73 (m, 2H), 2.56 (m, 2H), 2.05 (m, 1H), 1.97 (m, 1H), 1.73 (m, 5H), 1.54 (m, 3H), 1.01 (d, 3H).

The chemical industry reduces the impact on the environment during synthesis Methyl 2-bromopropanoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; Yi, Lin; Su, Xiping; Werth, Peter; (16 pag.)US2016/326113; (2016); A1;,
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