反应详情

In 1 ml of N,N-dimethylformamide was dissolved 100 mg of ethyl 2-[2-(2,4-difluorophenylamino)-5-fluoro-6-(2,4,6-trimethylbenzenesulfonyloxy)nicotinoyl]acetate, and 17 mg of ethanethiol and 28 mg of triethylamine were added thereto, after which the resulting mixture was subjected to reaction at room temperature for 4 hours. Subsequently, to the reaction mixture were added 3 ml of ethyl acetate and 3 ml of water, and the pH thereof was adjusted to 1.0 with 2N hydrochloric acid. The organic layer was separated, washed successively with 2 ml of water and 2 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and the residue thus obtained was purified by a column chromatography [Wako Silica Gel C-200, eluant: benzene-n-hexane (1:2 by volume)] to obtain 50 mg (yield 67.4%) of ethyl 2-[2-(2,4-difluorophenylamino)-6-ethylthio-5-fluoronicotinoyl]acetate. The physical properties of this compound were identical with those of the compound obtained in Example 19.

1. additionwere added
2. customafter which the resulting mixture was subjected to reaction at room temperature for 4 hours
3. customThe organic layer was separated
4. washwashed successively with 2 ml of water and 2 ml of saturated aqueous sodium chloride solution
5. dry with materialdried over anhydrous magnesium sulfate
6. customThe solvent was removed by distillation under reduced pressure
7. customthe residue thus obtained
8. customwas purified by a column chromatography [Wako Silica Gel C-200, eluant: benzene-n-hexane (1:2 by volume)]