反应详情

6.00 g of ethyl 2-chloro-4,4,4-trifluoroacetoacetate and 2.06 g of thioacetamide were dissolved in 30 ml of acetic acid and the mixture was refluxed for 6 hours with stirring. The resulting solution was neutralized with aqueous sodium bicarbonate solution, then extracted with ethyl acetate and the organic layer was concentrated. The residue was chromatographed on silica gel (eluent; n-hexane:chloroform:tetrahydrofuran=6:2:1 V/V) to obtain 3.7 g of ethyl 2-methyl-4-trifluoromethylthiazole-5-carboxylate (yield 56%).

1. temperaturethe mixture was refluxed for 6 hours
2. extractionextracted with ethyl acetate
3. concentrationthe organic layer was concentrated
4. customThe residue was chromatographed on silica gel (eluent; n-hexane:chloroform:tetrahydrofuran=6:2:1 V/V)