反应详情

Into 6 ml of N,N-dimethylformamide was suspended 0.18 g of sodium hydride (60% oily), and 0.44 g of 1,1,1-trifluoro-2-propanol was added at 10° C. After stirring for 10 minutes, 0.49 g of 4-chloro-6-methylpyridine-2-carbonitrile was added, the mixture was stirred for 1 hour, and the reaction solution was poured into an aqueous saturated ammonium chloride solution, followed by extraction with tert-butyl=methyl=ether. The organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.72 g of 6-methyl-4-(2,2,2-trifluoro-1-methylethoxy)pyridine-2-carbonitrile.

1. additionwas added at 10° C
2. stirringthe mixture was stirred for 1 hour
3. extractionfollowed by extraction with tert-butyl=methyl=ether
4. washwashed with an aqueous saturated sodium chloride solution
5. dry with materialdried with anhydrous magnesium sulfate
6. concentrationconcentrated