Tag: M.W=100-200

Adding a certain compound to certain chemical reactions, such as: 34846-90-7, name is Methyl 3-methoxyacrylate, 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 34846-90-7, Recommanded Product: 34846-90-7

Example 2 The toluene solution of 3-mercapto-2-butanone from the previous step (613 g of ca. 25 wtpercent solution) was placed in a clean, dry reactor along with 15 g of methyl-3-methoxyacrylate. The mixture was warmed to 25°C, stirred vigorously, and treated with solid sodium methoxide (8.5 g, ca. 0.1 equiv.) all at once. The remaining methyl-3-methoxyacrylate (151 g) was added in at a rate to keep the temperature at or below 35°C (2 h). The resulting mixture was allowed to reach room temperature and stir for 21 h. Concentrated hydrochloric acid (88 g) was added to the mixture over 30 min such that the temperature did not exceed 35°C. The resulting mixture was stirred vigorously for 2 h, then treated with 73 g of water, and stirred for 10 min more. The phases were allowed to separate. After standing for 10 min, the aqueous phase was drained from the reactor, and the upper, product phase was washed with 100 g of 5percent sodium bicarbonate solution. After being stirred for 15 min, the phases were allowed to separate. The lower, aqueous phase was drained from the reactor, and the upper. product phase was transferred to a distilling flask. The toluene was distilled through a 5-plate distillation column at 13.3 kPa [100 mmHg]. After a small fraction containing toluene and other low boiling impurities was collected, the product, 3-carbomethoxy-4,5-dimethylthiophene, was distilled through the column at 6.665 kPa [150 mmHg].

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-methoxyacrylate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Monsanto Technology LLC; EP1023283; (2003); B1;,
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These common heterocyclic compound, 18830-44-9, name is Methyl 3,3,3-trifluoropropanoate, 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. Recommanded Product: 18830-44-9

General procedure: R2BCl (2.0 mmol) was added dropwise to the solution of ester (1.0 mmol) and amine (3.0 mmol) in dichloromethane (3.5 mL) at -78 C and stirred at the same temperature for 1.5 h. Aldehyde (1.5 mmol) dissolved in dichloromethane was then added dropwise to the above reaction mixture and stirred at -78 C for 1 h and 0 C for 1 h. The reaction was quenched by the addition of pH 7 buffer solution (2 mL). The mixture was diluted with MeOH (2 mL), followed by the careful addition of 30% hydrogen peroxide (2 mL) and stirred vigorously for 4-5 h. The reaction mixture was partitioned between water (4 mL) and dichloromethane. The aqueous layer was extracted with dichloromethane (3 x 10 mL) and the combined organics were washed with brine (5 mL), dried (anhydrous Na2SO4), filtered, concentrated and purified by silica gel chromatography to obtain the pure aldol product.

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

Reference:
Article; Veeraraghavan Ramachandran; Gagare, Pravin D.; Parthasarathy, Gowrisankar; Tetrahedron Letters; vol. 52; 46; (2011); p. 6055 – 6057;,
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Reference of 23426-63-3,Some common heterocyclic compound, 23426-63-3, name is Methyl 2-bromo-2-methylpropanoate, molecular formula is C5H9BrO2, 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.

A mixture of 3-(3,3-dimethyl-6-trifiuoromethyl-l,2,3,4-tetrahydro-quinolin-2-yl)- phenylamine (1.5 g, 4.7 mmol), 2-bromo-2-methyl-propionic acid methyl ester (2.55 g, 14.1 mmol) and potassium carbonate (3.24 g, 23.5 mmol) in N, N-dimethylformamide (12 mL) was stirred at 25C for 5 d. Then the reaction mixture was extracted with ethyl acetate (2 x 100 mL), washed with water, dried over anhydrous sodium sulfate and concentrated in vacuo. Purification on flash silica gel chromatography (silica gel from QingDao, 200- 300 mesh, glass column from Shanghai SD company)(30% ethyl acetate/hexanes) to afford 2-[3-(3,3-dimethyl-6-trifiuoromethyl-l,2,3,4-tetrahydro-quinolin-2-yl)-phenylamino] -2- methyl-propionic acid methyl ester (400 mg, 20%) as a brown oil. LC/MS m/e calcd for C23H27F3N2O2 (M+H)+: 421.48, observed: 421.1.

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-bromo-2-methylpropanoate, its application will become more common.

Reference:
Patent; F. HOFFMANN-LA ROCHE AG; CHEN, Li; FENG, Lichun; HUANG, Mengwei; LIU, Yongfu; WU, Guolong; WU, Jim, Zhen; ZHOU, Mingwei; WO2011/128251; (2011); A1;,
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Application of 454-31-9, The chemical industry reduces the impact on the environment during synthesis 454-31-9, name is Ethyl 2,2-difluoroacetate, I believe this compound will play a more active role in future production and life.

Into a 250-mL 3-neck round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed 1,4-dibromobenzene (12.0 g, 50.8 mmol, 1.0 equiv) in THF (150.0 mL) at -78 C. Then n-butyllithium solution (1 M in hexane, 60.9 mL, 60.9 mmol, 1.2 equiv) was added at -78 C. The resulting mixture was stirred for 30 minutes at -78 C., and then ethyl 2,2-difluoroacetate (12.6 g, 101.5 mmol, 2.0 equiv) was added slowly at -78 C. The cooling bath was removed, and the resulting mixture was stirred for an additional 1 hour at room temperature. The reaction was then quenched by the addition of 50 mL water. The resulting mixture was extracted with ethyl acetate (250 mL*3), and the organic layers were combined, washed with brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was applied onto a silica gel column eluting with ethyl acetate/petroleum ether (1:10). This resulted in 7.6 g (64%) of 1-(4-bromophenyl)-2,2-difluoroethan-1-one as a light yellow semi-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, Ethyl 2,2-difluoroacetate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; Arvinas Operations, Inc.; Genentech, Inc.; Crew, Andrew P.; Wang, Jing; Berlin, Michael; Dragovich, Peter; Chen, Huifen; Staben, Leanna; US2019/300521; (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. 18830-44-9, name is Methyl 3,3,3-trifluoropropanoate, A new synthetic method of this compound is introduced below., category: esters-buliding-blocks

28.1. methyl 2-benzyl-4,4,4-trifluoro-3,3-dihydroxybutanoate To a solution of 675 mg (29.4 mmol) of sodium in 15 mL of anhydrous MeOH, under argon, are added dropwise 3.73 mL (29.4 mmol) of methyl 3,3,3-trifluoropropanoate. After stirring for 30 minutes at room temperature, 3.5 mL of benzyl bromide are added and the medium is heated for 12 hours at 70 C. The reaction mixture is then concentrated under reduced pressure. The residue obtained is taken up in 100 mL of EtOAc, washed with 50 mL of brine, dried over Na2SO4, filtered and concentrated under reduced pressure. After purification by chromatography on a column of silica gel, eluting with a cyclohexane/EtOAc mixture (85/15), 3.4 g of methyl 2-benzyl-4,4,4-trifluoro-3,3-dihydroxybutanoate are obtained in the form of an oil, which is used without further purification in the following step. Yield=37%.

The synthetic route of 18830-44-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; SANOFI; US2011/294788; (2011); 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 4891-38-7 as follows. Application In Synthesis of Methyl Phenylpropiolate

General procedure: Steroidal/nonsteroidal bromo vinyl aldehyde (0.5 mmol), alkyne (0.5 mmol), benzyl amine (0.5 mmol), Pd(OAc)2 (5 mol%), PPh3 (10 mol%), Na2CO3 (1.5 mmol) and neutral alumina (200 mg) were mixed intimately and the mixture was irradiated in a closed vessel in a Synthos 3000 microwave reactor at 600 Watt (140 C and 12 bar) for 10 min. After 10 min ethylacetate (30 mL) was added to the reaction mixture and it was filtered through whatman filter paper. The residue obtained after removal of ethylacetate layer was purified by silica gel column chromatography using EtOAc/hexane as the eluent to afford the pyridine derivative. The alumina on the filter paper was then dried in vacuo and can be used again for another two times in place of Pd(OAc)2 without substantial loss of the yield of the product.

According to the analysis of related databases, 4891-38-7, the application of this compound in the production field has become more and more popular.

Reference:
Article; Shekarrao, Kommuri; Nath, Dipankar; Kaishap, Partha Pratim; Gogoi, Sanjib; Boruah, Romesh C.; Steroids; vol. 78; 11; (2013); p. 1126 – 1133;,
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Synthetic Route of 85953-29-3, 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. 85953-29-3, name is Methyl 2-chloro-4-fluorobenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 1 : tert-butyl 4-((l-(3-chloro-4-(methoxycarbonyl)phenyl)piperidin-4-yl)methyl)piperidine- 1-carboxylate A mixture of methyl 2-chloro-4-fluorobenzoate (367 mg, 1.95 mmol), tert-butyl 4-(piperidin-4- y lmethyl)piperi dine- 1-carboxy late (500 mg, 1.77 mmol), and CS2CO3 (1269 mg, 3.89 mmol) in DMSO (8.8 ml) was degassed by bubbling with N2 and heated at 120C for lh under microwave condition. The mixture was diluted with EtOAc-H20, and the aq. layer was extracted with EtOAc (3x). The combined organic fractions were dried over Na2SC>4, filtered and the solvent was evaporated under reduced pressure. The reaction mixture was purified by ISCO column chromatography (silica gel ISCO 40 g prepacked column, eluting with 0-100% EtOAc/Hexane) to give the title compound (578 mg). LCMS m/z (M+H): Calc’d 451.2, found 451.4.

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-chloro-4-fluorobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; MERCK SHARP & DOHME CORP.; RUDD, Michael, T.; BENNETT, David Jonathan; WAI, Jenny; MENG, Zhaoyang; (257 pag.)WO2017/95758; (2017); A1;,
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Related Products of 2901-13-5, These common heterocyclic compound, 2901-13-5, name is Ethyl 2-methyl-2-phenylpropanoate, 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.

A solution – o’f 1 g- 2-methyl-2-phenyl-propionic acid ethyl ester in a mixture of 14 ml ‘sulfuric acid and 1 ml nitric acid was stirred at room temperature for 4 hours. The mixture was added to ice water and extracted with ethyl acetate. The organic layer wa’s washed with a satured aqueous solution of sodium hydrogen carbonate and dried over – anhydrous sodium sulfate. Filtration and concentration of the solvent under reduced pressure yielded a yellow solid;. The residue was purified- by, .flash chromatography on silica gel with a n-heptane/ dichloro-methane gradient. The fractions containing the product were combined and evaporated . to yield a yellow solid. Yield: 560 -mg.’- ‘ ‘ ‘M+H+. measured = ? ? ? ?1H-NMR’ (400 MHz, DMSO/TMS.)’1: ‘d = 8.69 (d, 1H) ; 8.5.3. (dd,’1H-); 8.10 ? (d, ‘1H) ; -”4 I 02 (q,–2H); 1.65 (s, 6H) ; ,1> 12 (t,

Statistics shows that Ethyl 2-methyl-2-phenylpropanoate is playing an increasingly important role. we look forward to future research findings about 2901-13-5.

Reference:
Patent; AVENTIS PHARMA S.A.; WO2006/10642; (2006); A1;,
Ester – Wikipedia,
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Electric Literature of 18469-52-8, A common heterocyclic compound, 18469-52-8, name is Methyl 4-(aminomethyl)benzoate, molecular formula is C9H11NO2, 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.

General procedure: To a solution of acid 3 (1.25 g, 3.1 mmol), HBTU (1.6 g, 3.7 mmol),and Et3N (10 mL) in 20 mL acetonitrile was added 1.2 equimolaramount of the appropriate amine. The mixture was kept stirring atroom temperature for 5 h. TLC detection found that the reactionwas complete, then the mixture was evaporated under reducedpressure to remove solvent. The residue was taken up saturatedsodium chloride and 1mL 3 N HCl and extracted with ethyl acetate(30 mL x 3), and the combined organic layers were washed twotimes with saturated sodium chloride and 1mL 3 N HCl. Theorganic layers were dried (MgSO4), filtered, and solvent wasremoved under reduced pressure at 40 C to give the crude product,which was purified by column chromatography to produce thecorresponding intermediate, 4 and 7.

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; Jia, Ruifang; Zhang, Jian; Ai, Wei; Ding, Xiao; Desta, Samuel; Sun, Lin; Sun, Zhuosen; Ma, Xiuli; Li, Zhong; Wang, Defeng; Huang, Bing; Zhan, Peng; Liu, Xinyong; European Journal of Medicinal Chemistry; vol. 178; (2019); p. 64 – 80;,
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Reference of 22223-49-0, 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. 22223-49-0, name is Methyl 2-amino-3-methylbenzoate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

Step 1. To a solution of 17 (15.0 g, 90.8 mmol) in DMF (200 mL) was added NBS (16.2 g, 90.8 mmol) at 0C. After addition, the mixture was warmed to 15C and stirred for 14 hours. The reaction mixture was quenched by addition of water (200 mL) and then extracted with ethyl acetate (3 x 250 mL). The combined organic phase was washed with water (3 x 250 mL) and brine (2 x 200 mL), dried over anhydrous Na2S04, filtered and concentrated in vacuo to give 18 (21.0 g) as a gray solid which was used directly in the next transformation. 1H NMR (CDC13, 400MHz) delta 7.90-7.89 (d, 1H), 7.29-7.28 (d, 1H), 5.84 (s, 2H), 3.87 (s, 3H), 2.15 (s, 3H); LCMS (ESI): m/z 246.0 (M+H).

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-amino-3-methylbenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; NUMERATE, INC.; RAIMUNDO, Brian; KOLTUN, Elena S.; GRIFFIN, John; STANGELAND, Eric; (50 pag.)WO2018/49328; (2018); A1;,
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