Esters-buliding-blocks

Reference of 623-47-2, 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. 623-47-2, name is Ethyl propiolate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

General procedure: To a solution of ethyl propiolate (98mg, 1.0mmol) in methanol (2mL), catalytic PtCl2 (5mg, 0.02mmol) was added. The mixture was stirred at 60C for 12h. The reaction solution was cooled to room temperature, and CH2Cl2 (20mL) was added. The mixture was then filtered, and the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel with hexane-ethyl acetate (20:1) as the eluent to give a mixture of (E)-ethyl 3-methoxyacrylate (4) and ethyl 3,3-dimethoxypropanoate (5) (112mg, 85% yield, 4_5=13:1, the ratio was determined by 1H NMR) as a colorless oil.

The synthetic route of Ethyl propiolate has been constantly updated, and we look forward to future research findings.

Reference:
Article; Chen, Qian; Zhang, Changyuan; Wen, Chunxiao; Fang, Jin; Du, Zhiyun; Wu, Dongling; Catalysis Communications; vol. 56; (2014); p. 101 – 105;,
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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. 34846-90-7, name is Methyl 3-methoxyacrylate, A new synthetic method of this compound is introduced below., Computed Properties of C5H8O3

Reference Production Example 1 (0548) A mixture of 21.1 g of methyl 3-methoxyacrylate, 10.0 g of hydrazine hydrate, and 20 mL of methanol was stirred with heating under reflux for 2 hours. The reaction mixture was concentrated under reduced pressure to obtain 11.0 g of 1H-pyrazol-3-ol. 1H-pyrazol-3-ol (0549) (0550) 1H-NMR (DMSO-d6) delta (ppm): 10.22 (1H, s), 7.35 (1H, d, J=2.2 Hz), 5.43 (1H, d, J=2.2 Hz)

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; SUMITOMO CHEMICAL COMPANY, LIMITED; HOU, Zengye; TAKAHASHI, Teruki; (156 pag.)US2016/174558; (2016); A1;,
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Reference of 99548-55-7, 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 99548-55-7 as follows.

A mixture of potassium acetate (649.2 mg, 6.55 mmol), 1,1?- bis(diphenylphosphino)ferrocene palladium dichloride (159.7 mg, 0.22 mmol),bis(pinacolato)diboron (1108.5 mg, 4.37 mmol) and methyl 4-bromo-2-methylbenzoate (500.0 mg, 2.18 mmol) in 1,4-dioxane (20 mL) was stirred at 110 ¡ãC for 4 h under N2 protection, and evaporated to dryness. The residue was taken up in EtOAc (30 mL), washed with water (20 mL x 2) and brine (20 mL), dried over Mg504 and concentrated. The residue was purified by flash column chromatography (10percent ethyl acetate in petroleum ether, Rf = 0.6) to afford methyl 2-methyl-4-(4,4,5 ,5-tetramethyl- 1,3 ,2-dioxaborolan-2-yl)benzoate (400 mg, 66.4percent yield) as a yellow oil.

According to the analysis of related databases, 99548-55-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; RQX PHARMACEUTICALS, INC.; GENENTECH, INC.; CHEN, Yongsheng; SMITH, Peter Andrew; ROBERTS, Tucker Curran; HIGUCHI, Robert I.; PARASELLI, Prasuna; KOEHLER, Michael F. T.; SCHWARZ, Jacob Bradley; CRAWFORD, James John; LY, Cuong Q.; HANAN, Emily J.; HU, Huiyong; YU, Zhiyong; (424 pag.)WO2017/84630; (2017); A1;,
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Synthetic Route of 13412-12-9,Some common heterocyclic compound, 13412-12-9, name is Methyl 3-(methylamino)but-2-enoate, molecular formula is C6H11NO2, 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.

Step 2: 2-(4-Bromo-benzoyl)-3-oxo-butyric acid methyl ester To 3-methylamino-but-2-enoic acid methyl ester (5.0 g, 39.1 mmol) in THF (100 mL) was added pyridine (3.7 mL, 47 mmol). The mixture was cooled to 0 C. and 4-bromobenzoyl chloride (8.55 g, 39.1 mmol) in THF (30 mL) was added dropwise over 2 minutes. The reaction was warmed to room temperature over 1 hour and stirred overnight. Aqueous workup provided the title compound.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route Methyl 3-(methylamino)but-2-enoate, its application will become more common.

Reference:
Patent; Amira Phamaceuticals, Inc.; US2011/82181; (2011); A1;,
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Reference of 792-74-5, 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. 792-74-5, name is Dimethyl [1,1′-biphenyl]-4,4′-dicarboxylate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A sample of 4,4′-biphenyldicarboxylate dimethyl ester, 2.0 g, was place in a 50 ml 2 neck 24/40 flask with stirring bar. Then trifluoroacetic acid, 10 ml, was added, and the mix was cooled to 0 0C. The cooled mixture was treated with 90% nitric acid, 0.38 ml, and then trifluoroacetic anhydride , 1.91 ml was added dropwise. TLC with 1 :8 ethyl acetate/hexanes on silica ant 30 minutes post TFAA showed some SM, and a new lower RF product. The mix was stirred 1 hour at 0 0C, then 3 hours at room temperature. The mixture was then poured into 100 ml of cold water, giving a gummy precipitate. The mix was treated with 80 ml of ethyl acetate and 20 ml of hexanes. The layers were separated, and the organic layer was washed with 100 ml of water. The organic layer was then stirred with 20 g of sodium bicarbonate in 100 ml of water. The ethyl acetate was evaporated in vacuo. The residue was treated with 100 ml of hexanes, heated to a boil, and diluted with ethyl acetate hot until a solution was obtained, then hexanes was added to a total volume of 200 ml. The mix was cooled to room temperature, and the resulting solids were collected by filtration, washed with 10 ml hexanes, and air dried to give 2-nitro-4,4′-biphenyldicarboxylate dimethyl ester, 1.319 g.NMR 500 MH D6DMS0: 8.51, d, J=IJ, IH, 8.31, dd, J=U, 8.1, IH, 8.06, dd, J=1.8, 8.3, 2H, 7.76, d, J=8, IH, 7.56, dd, J=1.8, 8.4, 2H, 3.94, s, 3H, 3.89, s, 3H

The synthetic route of Dimethyl [1,1′-biphenyl]-4,4′-dicarboxylate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; IMMUSOL INCORPORATED; WO2008/21745; (2008); A2;,
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Adding a certain compound to certain chemical reactions, such as: 106614-28-2, name is Methyl 2,4-difluorobenzoate, 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 106614-28-2, Product Details of 106614-28-2

To a solution of methyl 2, 4-difluorobenzoate (3.44 g, 20.00 mmol) in DMF (50 mL) was added 1H-pyrrolo [2, 3-b] pyridin-5-ol (2.70 g, 20.00 mmol) and K 2CO 3 (5.6 g, 40.00 mmol), the mixture was stirred at 80C for 20h. Cooled to room temperature, partitioned between EA (40 ml) and H 2O (40 mL), the aqueous layer was extracted with EA (20 mL). The combined organic layers were washed with H 2O (30 mL3), concentrated and purified by CombiFlash (0-60%, EA/PE) to give the crude product, which was crystallized from EA/PE=1/1 (50 mL) to give the isomer. The mother liquid was left standing over night, the precipitate was collected by filtration to give methyl 2- ((1H-pyrrolo [2, 3-b] pyridin-5-yl) oxy) -4-fluorobenzoate (600 mg) as a white solid. [M+1] + 286.9.

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 2,4-difluorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BEIGENE, LTD.; GUO, Yunhang; XUE, Hai; WANG, Zhiwei; SUN, Hanzi; (493 pag.)WO2019/210828; (2019); A1;,
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Reference of 37746-78-4,Some common heterocyclic compound, 37746-78-4, name is (E)-Ethyl 4-bromobut-2-enoate, molecular formula is C6H9BrO2, 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.

General procedure: A mixture of 1-(1H-pyrrol-2-yl) ethanone 1 (109 mg, 1.0 mmol), (E)-ethyl 4-bromobut-2-enoate 2 (256 mg, 1.0 mmol), and K2CO3 (414 mg, 3.0 mmol) in CH3CN (5 mL)was refluxed. The end of the reaction was monitored by the TLC. Ice water(100 mL) was poured into the mixture and CH2Cl2 (3 30 mL) was used toextract the mixture. The combined organic layers were dried over Na2SO4,filtered, and concentrated in vacuo. Purification by flash columnchromatography (Hexane/EtOAc = 10:1, v/v) afforded the desired product 7

The synthetic route of 37746-78-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Yang, Bingchuan; Huang, Zixiao; Guan, Hegen; Niu, Xiaoyi; Li, Yanqiu; Fang, Shuai; Ma, Chen; Tetrahedron Letters; vol. 54; 45; (2013); p. 5994 – 5997;,
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Electric Literature of 89-91-8, 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. 89-91-8, name is Methyl 2,2-dimethoxyacetate, This compound has unique chemical properties. The synthetic route is as follows.

Intermediate 55a: heptyl 2,2-bis(heptyloxy)acetate To a solution of methyl 2,2-dimethoxyacetate (5.0g, 37.3 mmol) in heptanol (26.3 ml_, 186 mmol) was added camphorsulfonic acid (0.43g, 1.86 mmol), and the reaction was heated to 100 C, overnight. The reaction was cooled to ambient temperature and concentrated under reduced pressure. The concentrate was purified on silica gel with dichloromethane / heptane as eluent to provide 4.0g of the desired compound. 1H NMR (400 MHz, CDCI3): delta = 4.86 (s, 1 H), 4.21 (t, J = 6.78 Hz, 2H), 3.52-3.69 (m, 4H), 1.55-1.77 (m, 6H), 1.20-1.45 (m, 24H), 0.82- 0.98 (m, 9H) ppm.

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

Reference:
Patent; NOVARTIS AG; BRITO, Luis; CHEN, Delai; GAMBER, Gabriel Grant; GEALL, Andrew; LOVE, Kevin; ZABAWA, Thomas; ZECRI, Frederic; WO2015/95346; (2015); 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. 20330-90-9, name is Dimethyl 5-chloroisophthalate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Safety of Dimethyl 5-chloroisophthalate

To a solution of 1,3-dimethyl 5-chlorobenzene-l ,3-dicarboxylate (4.00 g, 17.5 mmol) in dioxane (50 mL) and water (50 mL) was added NaOH (700 mg, 17.5 mmol). The resulting suspension was stirred vigorously at 40C for 2 hrs and then for a further 16 hrs at room temperature. The reaction mixture was evaporated to dryness, re-dissolved in water (-200 mL) and acidified to pH 3 using 1M HCl. The resulting white precipitate was sonicated for 2 mins and filtered. The white solid was washed further with water and then dried in a vacuum oven overnight. This afforded a white solid (3.6 g) which was a mixture of 3 products including 3-chloro-5-(methoxycarbonyl)benzoic acid. This solid was dissolved in DMF (150 mL) at 0C and diethylamine (2.56 g, 0.03 mol), DIPEA (6.09 ml, 0.03 mol) and HATU (6.64 g, 0.02 mol) were added. The reaction mixture was then stirred at room temperature for 6 hrs then evaporated to dryness, re- dissolved in EtOAc (200 mL) and washed with water (3 x 200 mL) and brine (2 X200 mL). The combined organics were then dried over MgSC>4 and evaporated to dryness to afford the crude product. This was purified by silica chromatography (Biotage: lOOg SNAP cartridge) eluting with 0-80% EtOAc in heptane to afford the title compound as a colourless oil (880 mg (28%); H NMR (500 MHz, CDC13) 5 1.13 (br. s, 3H), 1.26 (t, 3H), 3.24 (br.s, 2H), 3.54 (br. s, 2H), 3.93 (s, 3H),7.55 (m, 1H), 7.92 (m, 1H), 8.04 (m, 1H).

The synthetic route of 20330-90-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ACTIVE BIOTECH AB; FRITZSON, Ingela; LIBERG, David; EAST, Stephen; MACKINNON, Colin; PREVOST, Natacha; WO2014/184234; (2014); 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. 2051-59-4, name is 6-Chloro-2H-chromen-2-one belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Quality Control of 6-Chloro-2H-chromen-2-one

General procedure: A flame-dried reaction vessel with a magnetic stirring bar was sequentially charged with coumarin or p-dimethoxybenzene or 7-(2-Chloroethyl)theophylline (0.4mmol), PC (0.004mmol), pyridine N-oxide (0.82mmol, 78mg), CH2Cl2 (0.5mL) and CH3CN (0.5mL). Trifluoroacetic anhydride (0.8mmol, 168mg) was then added to the resulting homogeneous solution. The mixture was stirred at room temperature under irradiation from a blue LED. The solvent in the reaction mixture was removed under reduced pressure. The residue was redissolved in 2mL of CH3CN, and extracted 5 times with hexane (5mL each time). The PC was extracted into the hexane layer and separated for use in the next reaction. The CH3CN layer was dried with Na2SO4 and concentrated under vacuum. After separation and evaporation, the residue was purified by column chromatography on silica gel (200-300 mesh size) using petroleum ether/EtOAc as the eluent to give the trifluoromethyl coumarin.

The synthetic route of 2051-59-4 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Zhang, Xiaodan; Li, Yaming; Hao, Xinyu; Jin, Kun; Zhang, Rong; Duan, Chunying; Tetrahedron; vol. 74; 15; (2018); p. 1742 – 1748;,
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