Extracurricular laboratory: Synthetic route of 454-31-9

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

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