Month: June 2021

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 6065-82-3 as follows. SDS of cas: 6065-82-3

A solution of 40 ml (224 mmol) of ethyl diethoxyacetate, 19 ml (268 mmol) of acetyl chloride and 0.1 g (0.45 mmol) of iodine is heated at 50oC for 4 hours. Only 60% of the desired product is formed. The reaction medium is cooled to room temperature, 19 ml (268 mmol) of acetyl chloride are added and the medium is heated at 50oC for a further 18 hours. The reaction medium is evaporated to dryness under vacuum. 36.3 g (100%) of crude ethyl chloroethoxyacetate are obtained.

According to the analysis of related databases, 6065-82-3, the application of this compound in the production field has become more and more popular.

Reference:
Patent; GALDERMA RESEARCH & DEVELOPMENT, S.N.C.; WO2004/113331; (2004); 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. 15848-22-3, name is 5-Bromopentyl acetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Application In Synthesis of 5-Bromopentyl acetate

1- (4-METHOXY-PHENYL)-3-TRIFLUOROMETHYL-1, 4,5, 6-tetrahydro- pyrazolo [3,4-c] pyridin-7-one (0.500 g, 1.606 mmol) was dissolved in N, N- DIMETHYLFORMAMIDE (20 mL) and cooled to 0 OC. Sodium hydride (60%, 0.161 g, 4.016 mmol) was added followed by 5-BROMOPENTYL acetate (0.535 mL, 3.213 MMOL). The reaction was stirred at rt overnight, quenched with IN hydrochloric acid (100 mL), EXTRACTED WITH ETHYL ACETATE (3100 ML), WASHED WITH WATER (2X1100 L), washed with brine (1X100 mL), dried over MGSO4, concentrated, and purified by flash CHROMATOGRAPHY USING 0-100% ETHYL ACETATE/HEXANES gradient as the eluent to afford 6- [1- (4-METHOXY-PHENYL)-7-OXO-3-TRIFLUOROMETHYL-1, 4,5, 7-TETRAHYDRO- pyrazolo [3, 4-c] pyridin-6-yl]-hexanoic acid methyl ester (0.699 g, 99%). The ester (0.800 g, 1. 82 mmol) was dissolved in tetrahydrofuran (40 mL), 1M lithium borohydride (3.64 ML, 3.64 mmol) was added, and the reaction was refluxed overnight. The reaction was quenched with water (150 mL), extracted with ethyl acetate (3X150 ML), washed with brine (1X150 mL), dried over MGSO4, concentrated, and purified by flash chromatography using 0-100% ethyl ACETATE/HEXANES as the eluent to afford 0.478 g (64%): 1H NMR (CDCl3) 8 7.44 (d, j=8. 8 Hz, 2H), 6.96 (d, j=9.2 Hz, 2H), 3.84 (s, 3H), 3.67 (t, j=6. 8 Hz, 2H), 3.61 (t, j=6. 4 Hz, 2H), 3.47 (t, j=7. 5 Hz, 2H), 3.00 (t, j=6. 8 Hz, 2H), 1.65-1. 50 (m, 4H), 1.45-1. 30 (m, 4H) ppm.

The synthetic route of 15848-22-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BRYSTOL-MYERS SQUIBB COMPANY; WO2004/83177; (2004); A2;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 13671-00-6, These common heterocyclic compound, 13671-00-6, name is Methyl 2,6-difluorobenzoate, 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.

Reference Example 1 Synthesis of 1-(2,6-difluorophenyl)-2-(thiophen-2-yl)ethan-1-one To 100 ml of a THF solution containing 10.00 g of 2-(thiophen-2-yl)acetic acid was added dropwise 118.5 ml of a 1.9 mol/L THF solution of hexamethyldisilazane sodium at -78 C. and the mixture was stirred for 1 hour. Then, 20 ml of a THF solution containing 12.11 g of methyl 2,6-difluorobenzoate was added dropwise thereto, then, the temperature of the mixture was raised from -78 C. to room temperature and stirred for 2.5 hours. To the mixture was added an aqueous saturated ammonium chloride solution followed by stirring for 1 hour. Thereafter, ethyl acetate were added and the liquids were separated. The obtained organic layer was washed with saturated brine, and dried over magnesium sulfate. After the solvent was distilled off under reduced pressure, the obtained residue was purified by silica gel column chromatography. The title compound was obtained as 10.35 g of a red oily product. 1H-NMR (CDCl3) delta: 7.39 (1H, m), 7.22 (1H, m), 6.95 (4H, m), 4.36 (1H, s).

The synthetic route of 13671-00-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; MITSUI CHEMICALS AGRO, INC.; UMETANI, Hideki; OKAYA, Shun; IKISHIMA, Hideaki; FUKUMOTO, Takeshi; NISHIDA, Akihiro; YANAGI, Masanori; NAITO, Ryohei; MASUTOMI, Koji; SHIRAKAWA, Tomomi; SAKURADA, Akane; YUTANI, Satoshi; (368 pag.)US2020/45968; (2020); A1;,
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Reference of 394-35-4,Some common heterocyclic compound, 394-35-4, name is Methyl 2-fluorobenzoate, molecular formula is C8H7FO2, 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.

5-amino-4-methylpyrimidine (5g, 45 mmol) was dissolved in 200 mL THF and cooled to -20°C. A solution of n-BuLi (112.5 mmol) was added over 10 minutes and the solution was kept at -20°C for 30 min, then warmed to room temp and stirred for 3h. It was then cooled to -40°C and to it was added methyl-2-fluorobenzoate (1.75 mL, 13.7 mmol) and the solution stirred at -40°C for 30 min and then warmed to room temp for lh. 50 mL of methanol was then added over 5 min, followed by 6N aq HC1. The solution was stirred for 18h at room temp. It was then neutralized with NaHC03 to pH 8 and then diluted with ethyl acetate and water. The organics were washed with water three times and then brine and dried over sodium sulfate and concentrated in vacuo.The crude material was purified by flash chromatography using 10percent methanol/ DCM. 1.5 g of product was isolated as a yellow solid (16percent). 1H-NMR: (<3/4-DMSO, 400 MHz) delta 12.22 (s, 1H), 8.86 (s, 1H), 8.83 (s, 1H), 7.98(dt, 1H), 7.46 (m, 1H), 7.38 (m, 2H), 7.02(s, 1H) LC/MS: calculated for Ci2H8FN3: 213.2; found 214.10 (M+H)+. 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-fluorobenzoate, its application will become more common. Reference:
Patent; GILEAD SCIENCES, INC.; BJORNSON, Kyla; BONDY, Steven, S.; CHOI, You-chul; CHOU, Chien-hung; MISHRA, Ruchika; TRENKLE, James, D.; TSE, Winston, C.; VIVIAN, Randall, W.; WO2011/146817; (2011); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

These common heterocyclic compound, 136333-97-6, name is Methyl 4-(2-bromoethyl)benzoate, 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. Computed Properties of C10H11BrO2

EXAMPLE 13({[(1Z)-2,2-Diethyl-1-oxidohydrazono]amino}oxy)methyl 4-{2-[({2-chloro-5-[(2-methyl-2,3-dihydro-1H-indol-1-yl)carbamoyl]phenyl}sulphonyl)amino]ethyl}benzoateStep A: Methyl 4-{2-[(tert-butoxycarbonyl)({2-chloro-5-[(2-methyl-2,3-dihydro-1H-indol-1-yl)carbamoyl]phenyl}sulphonyl)amino]ethyl}-benzoateDissolve the compound obtained in Step A of Example 1 (1.04×10-2 mol) in acetonitrile (20 ml) and place the solution under stirring. Add diisopropylethylamine (1.24×10-2 mol) and then, after stirring for 10 minutes, intermediate 9 (2.20×10-2 mol) dissolved in acetonitrile (20 ml). Heat the mixture at 60 C. After 5 days, the reaction mixture is evaporated to dryness under reduced pressure. The residue obtained is chromatographed on a silica column using as eluant a 75/25 n-heptane/ethyl acetate mixture.The title product is obtained in the form of a pale yellow meringue.

The synthetic route of Methyl 4-(2-bromoethyl)benzoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LES LABORATOIRES SERVIER; US2010/286225; (2010); A1;,
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 41248-23-1 as follows. Recommanded Product: 41248-23-1

(1) cyclopentanone as raw material, the cyanohydrin reaction, the cyanide hydrolysis esterification to give hydroxycyclopentyl formate;(2) sulfonation reaction: synthesis of phenylacetyl chloride; docking ring reaction: the steps The resulting hydroxycyclopentanecarboxylic acid ethyl ester,Step (2) The resulting phenylacetyl chloride,Ethanol,After heating up,Slowly drop the concentration of 20%Ethanol sodium ethanol solution,After the reaction, ethanol was distilled off under reduced pressure,And then dropping the concentration of 20% hydrochloric acid,4-hydroxy-3-phenyl-1-oxaspiro [4.4] non-3-en-2-one obtained by filtration, the reaction equation is as follows:

According to the analysis of related databases, 41248-23-1, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ShandongOriental Pesticide Technology Industrial Co., Ltd; LI, YUAN; YU, LEXIANG; LI, LEI; SHI, LONGPING; SUN, FUJIANG; (27 pag.)CN106432163; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 13195-64-7, name is Diisopropyl malonate, 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 13195-64-7, name: Diisopropyl malonate

(1) Using 830 mmol of sodium hydride as a catalyst,200 mmol of diisopropyl malonate with440 mmol of propargyl bromide was added to the column210 mL of anhydrous acetonitrile in ice water bath,Stirring reaction for 8 hours,The product was washed with water,Extracted with ethyl acetate,Decompression spin dry,getBrownyellowSolid product,I.e. Compound 1;

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Diisopropyl malonate, and friends who are interested can also refer to it.

Reference:
Patent; Anhui Normal University; Hu Yimin; Xu Xiaoliang; (20 pag.)CN106866639; (2017); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Related Products of 252881-74-6, 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. 252881-74-6, name is tert-Butyl 3-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)propanoate, This compound has unique chemical properties. The synthetic route is as follows.

[00229j Synthesis of N- [(PEG)3-COO-t-Buj -N?-Boc-N?-methyl-ethylene-diamine.To the solution of t-Bu-(PEG)3-amine (1 .01 g , 3.64 mmol) in 20 ml of methanol, (N-methyl)-N-Boc acetaldehyde(0.63 g, 3.64 mmol) was added. The mixture was stirred at room temperature for 3 hours. NaBH4 (0.412g, 10.9 mmol) was added to the mixture at 0C, and the resultant mixture was stirred at 0 C for 1 hour and 1 hour at room temperature. The reaction was quenched by adding 5 ml of water. After removal of solvent, 5 ml of water was added, and the mixture was extracted three times with methylene chloride. The combined organic layer was dried over Na2SO4, and the product was purified by flash silica chromatography using heptane/ethyl acetate to methylene chloride/methanol to give a yield of 72% (1.14 g). ?H NMR (300 MHz, CD2C12) oe ppm: 3.68 (t, 2H, OCH2), 3.56-3.60 (br, 1OH, CH2), 3.53 (t, 2H, OCH2), 3.29 (t, 2H, CH2), 2.85 (s, 3H, NCH3), 2.7-2.8 (m, 4H, NCH2), 2.47 (t, 2H, COCH2), 1.44 (s, 18H, CH3); MS-ESI (mle):435.5 [M+H].

The chemical industry reduces the impact on the environment during synthesis tert-Butyl 3-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)propanoate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; PROMEGA CORPORATION; MUSTAFA, Dana; ZHOU, Wenhui; MEISENHERMIER, Poncho; DUELLMAN, Sarah; MA, Dongping; CALI, James, J.; WO2015/116867; (2015); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Reference of 6091-64-1, These common heterocyclic compound, 6091-64-1, name is Ethyl 2-bromobenzoate, 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.

Ethyl 2-bromobenzoate (1g, 4.37mmol) prepared from Step 1 wasdissolved in toluene (20 mL) and ethanol (4mL) mixed solution, and then theretowere added 4-fluorophenyl boronic acid (672mg, 4.80mmol), potassium carbonate(1.21g, 8.73mmol) and tetrakis (triphenylphosphine) palladium (504mg,0.44mmol). The reaction was stirred at 100 deg. C 6 hours, cooled to roomtemperature and filtered through Celite. The reaction was concentrated underreduced pressure to remove the solvent. Then washed with water and extracted ethyl acetate. Theorganic layer was dried over anhydrous magnesium sulfate, filtered andconcentrated. The resulting residue was purified by column chromatography toproduce the title compound (948mg, 89%).

Statistics shows that Ethyl 2-bromobenzoate is playing an increasingly important role. we look forward to future research findings about 6091-64-1.

Reference:
Patent; East Asia ST Corporation; Jin, Shunhui; Ren, Yuanbin; Cao, Zonghuan; Cui, Shangao; Pu, Zhengxiang; Jin, Miyan; Cui, Chenghe; Lee, Mingjing; Zhao, Kangxun; (182 pag.)CN105555761; (2016); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Synthetic Route of 35450-36-3, A common heterocyclic compound, 35450-36-3, name is Methyl 2-bromo-5-methoxybenzoate, molecular formula is C9H9BrO3, 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.

Add CuI (19.45 mg), PdCl2 (PPh3) 2 (105.29 mg) to the round bottom flask,Under nitrogen, methyl 2-bromo-5-methoxybenzoate (1.68 mL), phenylacetylene (0.66 mL), Et3N (2.08 mL), and THF (15 mL) were added in this order, and the reaction was performed at 55 C for 6 h.TLC tracks the progress of the reaction; after the reaction is complete, the resulting reaction solution is cooled to room temperature,Then filtered through diatomaceous earth and purified by column chromatography to obtain the first intermediate;Dissolving the first intermediate in methanol, adding a 10% NaOH solution, and stirring at room temperature for 2 h,TLC tracks the progress of the reaction; after the reaction is complete, adjust the pH of the resulting reaction solution to dilute 2-3 with dilute hydrochloric acid,The obtained solid was filtered and purified by recrystallization to obtain a second intermediate;Add SOCl2 to the second intermediate and reflux at 90 C for 2 h.TLC followed the progress of the reaction; after the reaction was completed, SOCl2 was removed to obtain a third intermediate;At 0 C, add N-methoxyamine and potassium carbonate to 15 mL of ethyl acetate in this order.(EA) and water (EA: water volume ratio = 2: 1), the third intermediate was added dropwise after 10 min, and the reaction was performed at room temperature for 1 h.TLC tracks the progress of the reaction; after the reaction is complete, it is extracted with EA and H2O.Dry over anhydrous sodium sulfate and recrystallize to obtain N-methoxy-5-methoxy-2-phenylethynylbenzamide (1h);

The synthetic route of 35450-36-3 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Hunan University of Science and Technology; Xie Wenlin; Liu Renzhi; Qiu Guanyinsheng; (15 pag.)CN110590641; (2019); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics