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. Quality Control of Ethyl 2,2-difluoroacetate
Step 1: Preparation of 1-ethoxy-2,2-difluoroethanol To a solution of ethyl 2,2-difluoroacetate (200 g, 1.59 mol) in tert-butyl methyl ether (1200 mL) was added LiAlH4 (33 g, 0.78 mol) portionwise at 78 C. under a nitrogen atmosphere. Once the addition was complete, the reaction mixture was continually stirred for 6 hrs at 78 C. EtOH (75 mL, 98%) was added dropwise to quench the reaction at 78 C., and the resulting mixture was allowed to warm to rt. The mixture was poured into ice/water, and concentrated H2SO4 (100 mL) was added carefully with stirring. The mixture was extracted with tert-butyl methyl ether (two*1 L) and the combined organic layers were washed with water, dried over Na2SO4, and concentrated to afford crude material that was submitted to distillation under reduced pressure. The fraction was collected at 45-55 C./-0.1 MPa to afford the title compound (75 g, 37% yield) as a colorless liquid.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 454-31-9, its application will become more common.
Reference:
Patent; PFIZER INC.; Cheng, Hengmiao; Johnson, JR., Theodore Otto; Kath, John Charles; Liu, Kevin Kun-Chin; Lunney, Elizabeth Ann; Nagata, Asako; Nair, Sajiv Krishnan; Planken, Simon Paul; Sutton, Scott Channing; US2013/79324; (2013); A1;,
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