反应详情

A mixture of 0.08 g of 2,2-bis(fluoromethyl)-N-methyl-6-nitro-2H-1-benzopyran-4-carboxamide, 0.06 g of a Lawesson's reagent and 2 ml of benzene was refluxed with heating for 1 hour. The solvent was distilled. The resultant residue was purified according to silica gel column chromatography (developing solution:CH2Cl2) and further recrystallized by a mixed solvent of ethyl acetate and hexane to obtain 71 mg of 2,2-bis(fluoromethyl)-N-methyl-6-nitro-2H-1-benzopyran-4-carbothioamide with a melting point of 134°-135° C.

1. temperaturewas refluxed
2. temperaturewith heating for 1 hour
3. distillationThe solvent was distilled
4. customThe resultant residue was purified
5. customfurther recrystallized by a mixed solvent of ethyl acetate and hexane