F[C:2]([N:7](C)C)(F)[CH:3]([F:5])[F:4].B(F)(F)F.CN([C:17](=[CH2:23])[C:18]([O:20][CH2:21][CH3:22])=[O:19])C.[CH3:24][NH:25]N>C(#N)C>[F:5][CH:3]([F:4])[C:2]1[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:23][N:25]([CH3:24])[N:7]=1
10.8 g of N-1,1,2,2-tetrafluoroethyldimethylamine were initially charged in 50 ml of acetonitrile under argon and 26 g of boron trifluoride as a 17% solution in CH3CN were added at RT. The mixture was stirred for 30 min and then admixed with 8.67 g of ethyl dimethylaminoacrylate. The mixture was stirred at RT for 2 h and then added slowly to the solution of 3.4 g of methylhydrazine in 10 ml of acetonitrile at 10° C. After stirring at RT for 2 h, the acetonitrile was removed completely under reduced pressure and the product was admixed with water and filtered off. Distillation under reduced pressure or washing with cyclohexane afforded 10 g of the product with the purity of 99% and an m.p. of 62-63° C.
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