Tag: M.W=100-200

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. 18595-14-7, name is Methyl 4-amino-3-methylbenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below. Recommanded Product: 18595-14-7

To a stirred and cooled (0 C) slurry of commercially available methyl 4-amino-3-methylbenzoate (2 g, 12.12 mmol) in 6 N HCl (12 mL) was added NaNO2 (0.92 g, 13.33 mmol) in water (2 mL) drop wise maintaining a temperature of <15 C during the addition. The mixture was stirred an additional 1.5 h affording a light yellow, homogeneous solution. To the mixture was carefully added 4.58 g (24.24 mmol) of anhydrous SnCl2. The temperature during the addition was kept <10 C. The mixture was stirred at 0 C for 1 h. The precipitated solid was collected by filtration, dried under vacuum to afford methyl 4-hydrazinyl-3-methylbenzoate hydrochloride 4 (1.75 g 81%) as a brown solid: mp 224-226 C; 1H NMR (CDCl3, 500 MHz) delta ppm 2.22 (s, 3H), 3.80 (s, 3H), 6.99 (d, J = 8.5 Hz, 1H), 7.70 (s, 1H), 7.77 (d, J = 8.5 Hz, 1H); MS (ESI): m/z calcd for C9H12N2O2 ([M+H]+) 181.0932; found 181.0911 ([M+H]+). The synthetic route of 18595-14-7 has been constantly updated, and we look forward to future research findings. Reference:
Article; Chiruta, Chandramouli; Zhao, Yanrong; Tang, Fangling; Wang, Tao; Schubert, David; Bioorganic and Medicinal Chemistry; vol. 21; 10; (2013); p. 2733 – 2741;,
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These common heterocyclic compound, 1188911-72-9, name is Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate, 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. Quality Control of Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate

[00444] To a -78 C solution of diisopropylamine (15 mL, 107 mmol) in THF (150 mL) was added n-BuLi (2.4 mol/L, 8 mL) dropwise. The reaction mixture was stirred for 30 minutes and a solution of methyl 3,3,3-trifluoro-2,2-dimethylpropanoate (3 g, 17.63 mmol) in acetonitrile (10 mL, 239 mmol) was added dropwise slowly. One hour later, the mixture was warmed slowly to rt and stirred for 2 hours. The mixture was quenched with saturated aqueous ammonium chloride solution (50 mL), and the resulting mixture was extracted with ethyl acetate (300 mL), dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated in vacuo and the residue was purified by silica gel column chromatography (EtOAc/PE (v/v) = 1/1) to give the title compound as a white solid (1.53 g, 48%). The compound was characterized by the following spectroscopic data: MS-ESI: (ESI, pos.ion) m/z: 180.1 [M+lfb; and ?H NMR (600 MHz, CDC13) 3.77 (s, 2H), 1.43 (s, 6H).-78 C

The synthetic route of Methyl 3,3,3-trifluoro-2,2-dimethylpropanoate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SUNSHINE LAKE PHARMA CO., LTD.; CHENG, Changchung; ZHANG, Yingjun; LIU, Bing; LONG, Bohua; CHEN, Yu; CHENG, Zhixin; (182 pag.)WO2016/8433; (2016); A1;,
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Electric Literature of 1128-76-3, 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. 1128-76-3, name is Ethyl 3-chlorobenzoate, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: The ethyl esters (0.15 mol; 2a-o) were taken in 250 mL round bottom flask.About 30 mL of methanol was added to the flask and homogenized by stirringat room temperature. Hydrazine hydrate (80%; 0.15 mol) was introduced to theflask drop wise and the reaction apparatus was refluxed for 5-6 hrs. Reactionprogress was confirmed by thin layer chromatography. n-Hexane and ethylacetate (3:2). At the end of reaction, excess of solvent was evaporated andresidue was poured into the ice cold water. Precipitates of acid hydrazides werefiltered, washed with water and dried. Re-crystallization of acid hydrazides wasperformed by using methanol.

The chemical industry reduces the impact on the environment during synthesis Ethyl 3-chlorobenzoate. I believe this compound will play a more active role in future production and life.

Reference:
Article; Aziz-Ur-Rehman; Ahtzaz, Samreen; Abbasi, Muhammad Athar; Siddiqui, Sabahat Zahra; Rasool, Shahid; Ahmad, Irshad; Journal of the Chilean Chemical Society; vol. 62; 1; (2017); p. 3370 – 3375;,
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Reference of 7424-91-1, A common heterocyclic compound, 7424-91-1, name is Methyl 3,3-dimethoxypropanoate, molecular formula is C6H12O4, 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.

Example 2: Preparation of methyl 3-methoxyprop-2-enoate Under an atmosphere of nitrogen, 0.2 g (2 mmol) of methanesulfonic acid (Fluka) was added to 150 g of a filtrate, analogously obtained as described in example 1 (about 85percent, 0.86 mol of methyl 3,3-dimethoxypropionate), in a distillation apparatus with round-bottomed flask. Under constant flow of nitrogen, the mixture was slowly heated to 160 ¡ãC, and the methanol formed was directly distilled off. After 6 hours, the heat supply was stopped. The methyl 3-methoxy- prop-2-enoate obtained in this manner was 88percent pure (GC) and was purified by rectification at 10 kPa. The yield was 85 g (85percent) of methyl 3-methoxyprop-2-enoate (Ki0 kpa = 950C) with a purity of 99percent (GC).; Example 6: Preparation of methyl 3-methoxyprop-2-enoate After distillative removal of the unreacted trimethyl ortho formate from example 1, 4.4 t (30 kmol) of the methyl 3,3-dimethoxypropionate thus obtained were reacted under an atmosphere of nitrogen with 6 kg (62 mol) of methanesulfonic acid analogously to example 2. Rectification at 10 kPa gave 2.4 t (21 kmol, 69percent based on trimethyl orthoformate employed) of methyl 3-methoxyprop-2-enoate (Ki0 kpa = 95 ¡ãC) in a purity of 93percent (GC).

The synthetic route of 7424-91-1 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LONZA AG; WO2009/56293; (2009); A1;,
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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., SDS of cas: 2065-23-8

To the methyl phenoxyacetate obtained by distillation, 0.09 g of lead acetate having a purity of 99% and1.29g of 99% pure 2,3,4-trichlorothiophene, added 118.34g at 20 C99% pure thionyl chloride is reacted, and the reaction is kept at this temperature for 0.5 h, and distilled at a pressure of 1 kPa to collect a fraction of 110 to 120 C.The methyl 4-chlorophenoxyacetate was obtained in an amount of 200.87 g, and the content was 98.84%.

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; Chi Zhilong; Zhang Liguo; Hu Yishan; (15 pag.)CN108947822; (2018); A;,
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Application of 431-47-0, 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. 431-47-0 name is Methyl 2,2,2-trifluoroacetate, 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.

e) 2,2,2-Trifluoro-N-prop-2-ynyl-acetamide To 15 g (272.3 mmol) propargylamine in 275 ml anhydrous methanol 36.6 g (285.9 mmol) methyl trifluoroacetate were added with cooling. The resulting reaction mixture was stirred for an additional four hours at room temperature. Afterwards the solvent was removed by distillation at reduced pressure. The residue was dissolved in 300 ml trichloromethane and extracted four times, twice each with 300 ml of a saturated sodium bicarbonate solution and twice each with 300 ml water. The separated organic phase was dried over magnesium sulfate, filtrated and the solvent was removed by distillation (yield: 23.3 g).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, Methyl 2,2,2-trifluoroacetate, and friends who are interested can also refer to it.

Reference:
Patent; Roche Diagnostics GmbH; F.HOFFMANN-LA ROCHE AG; EP1842923; (2007); A1;,
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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 17994-94-4 as follows. Recommanded Product: 17994-94-4

General procedure: To a mixture of aldehyde (1 mmol) and amine/amine hydrochloride (1 mmol) in anhydrous CH2Cl2 (10 mL) was added triethylamine (2.5 mmol) at rt, and the resulting solution was stirred vigorously for 1 h. To this was then added (Boc)2O (1.2 mmol) followed by sodium triacetoxyborohydride (2 mmol). The reaction was stirred for an additional 4 h at rt, quenched with saturated NaHCO3 solution, and extracted with CH2Cl2. The combined organic fractions were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. The crude residue was purified by flash chromatography (95:05?50:50, hexanes/EtOAc) to afford the N-Boc secondary amine. Most of the title compounds were present as a mixture of rotational isomers in their 1H and 13C NMR spectra.

According to the analysis of related databases, 17994-94-4, the application of this compound in the production field has become more and more popular.

Reference:
Article; Neelarapu, Raghupathi; Petukhov, Pavel A.; Tetrahedron; vol. 68; 35; (2012); p. 7056 – 7062;,
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Electric Literature of 52449-43-1, 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. 52449-43-1, name is Methyl 4-chlorophenylacetate, This compound has unique chemical properties. The synthetic route is as follows.

Referential Example 2 Methyl (4-chlorophenyl)bromoacetate To a solution of 102 g (0.55 mole) of methyl (4-chlorophenyl)acetate in 100 ml of carbon tetrachloride was added 97.9 g (0.55 mole) of N-bromosuccinimide. The resulting mixture was refluxed and irradiated with a 500 W bromo lamp for 5 hours. It was then cooled, filtered, and the filtrate was evaporated to dryness to give 150 g (103% yield) of methyl (4-chlorophenyl)bromoacetate. NMR (CDCl3) delta ppm; 3.79 (3H, s), 5,31 (1H, s), 7.3-7.7 (4H, s)

The chemical industry reduces the impact on the environment during synthesis Methyl 4-chlorophenylacetate. I believe this compound will play a more active role in future production and life.

Reference:
Patent; SUMITOMO PHARMACEUTICALS COMPANY, LIMITED; SUMITOMO CHEMICAL COMPANY, LIMITED; EP256687; (1991); B1;,
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Electric Literature of 17994-94-4, The chemical industry reduces the impact on the environment during synthesis 17994-94-4, name is Methyl 7-aminoheptanoate hydrochloride, I believe this compound will play a more active role in future production and life.

Methyl 7-(4-(l^-dioxo-l,3-bis(quinolin-8-ylamino)pr pan-2-yl)benzamido)heptanoate, 60.; To compound 59 (200 mg, 0.42 mmol) in (?(? (20 mL) at rt added 7-aminoheptanoic acid methyl ester (as the hydrochloride, 90 mg, 0.46 mmol), Et^ (47 mg, 0.46 mmol) and EDC (89 mg, 0.46 mmol). The mixture was allowed to stir at rt for 12 h. Water was added and the mixture was worked up with Combined organic extracts were dried with anhydNa2S04, solvent removed under vacuum and the residue was purified by column chromatography (silica gel 230-400 mesh, 80% ethyl acetate in hexanes as the eluent) to afford 70 as a white solid (202 mg, 78%).Mp = 178-180 C. NMR (300 MHz, CDC13): delta = 1.34-1.36 (m, 4 H), 1.59-1.62 (m, 4 H), 2.29 (t, 2 H, J = 5.7 Hz), 3.42 (m, 2 H), 3.64 (s, 3 H), 5.03 (s, 1 H), 6.14 (s, 1 H), 7.43-7.47 (m, 2 H), 7.53 (d, 4 H, J = 3.3 Hz), 7.84 (dd, 4 H, /, = 6.3 Hz, J2 = 15.3 Hz), 8.15 (d, 2 H, J = 6 Hz), 8.82-8.86 (m, 4 H), 10.98 (s, 2 H). I3C NMR (75 MHz, CDC13): delta = 24.7, 26.5, 28.7, 29.4, 33.9, 40.0, 51.5, 62.3, 117.1, 121.7, 122.4, 127.1, 127.9, 128.7, 134.1, 134.8, 136.2, 138.0, 138.7, 148.7, 166.6, 167.0, 174.2. HRMS (FAB+) Calcd for C36H36O5N5 = 618.2638, Found = 618.2712.

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 7-aminoheptanoate hydrochloride, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; THE TRUSTEES OF COLUMBIA UNIVERSITY IN THE CITY OF NEW YORK; SLOAN-KETTERING INSTITUTE FOR CANCER RESEARCH; BRESLOW, Ronald; MARKS, Paul, A.; ABHILASH, K., G.; WANG, Jianing; WO2011/146855; (2011); A1;,
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Electric Literature of 57486-67-6, A common heterocyclic compound, 57486-67-6, name is Methyl 2-(2-fluorophenyl)acetate, molecular formula is C9H9FO2, 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.

1-tert-butyl 4-methyl 4-(2-fluorophenyl)piperidine-1,4-dicarboxylate. A flask was charged with sodium hydride (2.14 g, 89.2 mmol) and dimethylformamide (70 ml) at 0 C. under nitrogen. Methyl 2-(2-fluorophenyl)acetate (5 g, 29.7 mmol) was added to the flask, and after stirring for 25 min, tert-butyl bis(2-chloroethyl)carbamate (8.6 g, 35.6 mmol) was added. The reaction was allowed to warm to rt and stirred overnight. The reaction was quenched with a saturated solution of ammonium chloride and extracted with ethyl acetate (5¡Á100 mL). The organics were collected, washed with brine, dried over sodium sulfate, and concentrated in vacuo. The residue was purified via silica gel chromatography (10/90?50/50 ethyl acetate/hexanes) to yield 1.7 g (17%) of the desired product. 1H-NMR (CDCl3, 400 MHz) delta ppm 7.29 (m, 1H), 7.24 (m, 1H), 7.12 (m, 1H), 7.00 (m, 1H), 3.86 (m, 2H), 3.67 (m, 3H), 3.22 (m, 2H), 2.37 (m, 2H), 1.96 (m, 2H), 1.44 (s, 9H). Mass spec.: 360.22 (MNa)+. LC tr=3.503 min (Phenomenex-Luna 4.6¡Á50 mm S10, 10% MeOH/90% H2O/0.1% TFA?90% MeOH/10% H2O/0.1% TFA Gradient Time=4 min, Flow rate=4 mL/min)

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

Reference:
Patent; Bristol-Myers Squibb Company; US2007/249607; (2007); A1;,
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