Category: 454-31-9

Electric Literature of 454-31-9,Some common heterocyclic compound, 454-31-9, name is Ethyl 2,2-difluoroacetate, molecular formula is C4H6F2O2, 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 Preparation of 4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)-butane-1,3-dione Ethyl difluoroacetate (4.06 g, 32.7 mmol) was dissolved in methyl tert-butyl ether (50 mL). To the stirred solution was added 25 weight % sodium methoxide (7.07 g, 32.7 mmol) followed by 3′-fluoro-4′-methoxyacetophenone from Step 1 (5.0 g, 29.7 mmol). After stirring for 16 hours, 1N HCl (50 mL) was added. The organic layer was collected and washed with water (2*50 mL), dried over anhydrous MgSO4, filtered, and added to hexanes to precipitate a tan solid (7.0 g, 96%): mp 70-72 C.

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

Reference:
Patent; G. D. Searle & Co.; US6376528; (2002); B1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Adding a certain compound to certain chemical reactions, such as: 454-31-9, name is Ethyl 2,2-difluoroacetate, 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 454-31-9, Recommanded Product: 454-31-9

To a solution of 1-bromo-4-iodobenzene (28.3 g, 0.100 mol) in anhydrous THF (300 mL) at -78 was added n-BuLi (2.5 M, 44.0 mL, 0.110 mol) , and the resulting mixture was stirred for 30 min before ethyl 2, 2-difluoroacetate (13.6 g, 0.110 mol) was added dropwise. After the addition, the mixture was stirred at -78 for 1 h, then excess base was quenched with aqueous 1N HCl solution (80 mL) . The product mixture was warmed to ambient temperature and extracted with MTBE (400 mL ¡Á 3) . The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and concentrated to afford the title compound. MS: m/z 236.2 (M + 1) .1H NMR (400 MHz, DMSO-d6) delta 7.96 (d, J 8.0 Hz, 2H) , 7.85 (d, J 8.0 Hz, 2H), 7.28 -7.02 (m, 1H) .

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; MERCK SHARP & DOHME CORP.; COOKE, Andrew J.; PITTS, Daniel; JOHNSON, Adam; BESHORE, Douglas C.; HURZY, Danielle; MITCHELL, Helen; FRALEY, Mark; MCCOMAS, Casey; SCHIRRIPA, Kathy; MERCER, Swati P.; NANDA, Kausik; MENG, Dongfang; WU, Jane; BABAOGLU, Kerim; LI, Chun Sing; MAO, Qinghua; QI, Zhiqi; (156 pag.)WO2016/54807; (2016); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 454-31-9, name is Ethyl 2,2-difluoroacetate, A new synthetic method of this compound is introduced below., Recommanded Product: Ethyl 2,2-difluoroacetate

Step 2 Preparation of 4,4-difluoro-1-(3-fluoro-4-methoxyphenyl)-butane-1,3-dione Ethyl difluoroacetate (4.06 g, 32.7 mmol) was dissolved in methyl t-butyl ether (50 mL). To the stirred solution was added 25 weight % sodium methoxide (7.07 g, 32.7 mmol) followed by 3′-fluoro-4′-methoxyacetophenone (5.0 g, 29.7 mmol). After stirring for 16 hours, 1N HCl (50 mL) was added. The organic layer was collected and washed with water (2*50 mL), dried over anhydrous MgSO4, filtered, and added to hexanes to precipitate a tan solid (7.0 g, 96%): mp 70-72 C.

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; Isakson; Peter C.; Anderson; Gary D.; Gregory; Susan A.; US5700816; (1997); A;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

Electric Literature of 454-31-9, 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. 454-31-9, name is Ethyl 2,2-difluoroacetate belongs to esters-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.

A mixture of intermediate 2 (20 g, 0.088 mol) in benzene (200 mL) was stirred at 0 C under nitrogen atmosphere. Potassium tert-butoxide (12 g) followed by ethyl difluoroacetate (13.14 g, 0.106 mol) were added at 0-5 C. The reaction mixture was stirred at rt for 5 h. Then 10% H2SO4 (10 mL) was added dropwise until pH = 7 keeping the temperature at 15-20 C by cooling. The mixture was extracted with EtOAc (2 x 50 mL). The organic layer was separated and washed with brine (2 x 20 mL), dried (MgS04), filtered and evaporated in vacuo yielding intermediate 13 (26 g, 97%).

The synthetic route of Ethyl 2,2-difluoroacetate has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; BARTOLOME-NEBREDA, Jose Manuel; TRABANCO-SUAREZ, Andres Avelino; ALCAZAR-VACA, Manuel Jesus; (192 pag.)WO2018/154133; (2018); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics

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. 454-31-9, name is Ethyl 2,2-difluoroacetate, A new synthetic method of this compound is introduced below., Recommanded Product: 454-31-9

Intermediate 6 (53.35 g, 0.22 mol) was stirred in toluene (1500 mL) at 0 C under N2. Potassium tert-butoxide (34.14 g) was added at 0-5 C and 2,2-difluoro-acetic acid ethyl ester (33.01 g, 0.27 mol) was added dropwise at 0-5 C. The RIVI was stirred at RT for 2 h, then washed with 10% H2S04 in water and the OL was dried on MgSO4,filtered and evaporated, yielding intermediate 7 (70.50 g, quantitative).

The synthetic route of 454-31-9 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; VAN ROOSBROECK, Yves, Emiel, Maria; BUIJNSTERS, Peter, Jacobus, Johannes, Antonius; TRESADERN, Gary; JACOBY, Edgar; OEHLRICH, Daniel; GIJSEN, Henricus, Jacobus, Maria; (67 pag.)WO2018/83103; (2018); A1;,
Ester – Wikipedia,
Ester – an overview | ScienceDirect Topics