反应详情

Tetrabutylammonium cyanide (18.5 g, 67 mmol) was added to a solution of 5-chloromethyl-4-methyl-2-(4-trifluoromethyl-phenyl)-thiazole [15.0 g, 51 mmol; PCT Int. Appl. (2002), WO 0292590 A1] in acetonitrile (340 ml). The solution was stirred at ambient temperature for 16 h, saturated aqueous sodium bicarbonate solution/ice water 1/1 and ethyl acetate were added and the layers were separated. The aqueous layer was extracted with ethyl acetate, the combined organic layers were washed with ice water/brine 1/1, dried over sodium sulfate and the solvent was evaporated in vacuo to give a brown oil which was purified by column chromatography (silica gel, n-heptane/CH2Cl2) to yield 8.58 g (30 mmol, 59%) of the title compound as light yellow solid.

1. customthe layers were separated
2. extractionThe aqueous layer was extracted with ethyl acetate
3. washthe combined organic layers were washed with ice water/brine 1/1
4. dry with materialdried over sodium sulfate
5. customthe solvent was evaporated in vacuo
6. customto give a brown oil which
7. customwas purified by column chromatography (silica gel, n-heptane/CH2Cl2)