反应详情

In 39 ml of N,N-dimethylformamide was dissolved 3.89 g of methyl 2-(2,4-difluorophenylamino)-5-fluoro-6-(mesitylenesulfonyloxy)nicotinate, and to the resulting solution were added 1.34 g of thiophenol and 1.23 g of triethylamine, after which the resulting mixture was subjected to reaction at room temperature for 5 hours. Subsequently, 120 ml of ethyl acetate and 120 ml of water were added to the reaction mixture, and the pH of the mixture was adjusted to 2.0 with 2N hydrochloric acid. The organic layer was separated, washed successively with 80 ml of water and 80 ml of saturated aqueous sodium chloride solution, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 20 ml of n-hexane, after which the crystals thus deposited were collected by filtration to obtain 2.85 g (yield 90.2%) of methyl 2-(2,4-difluorophenylamino)-5-fluoro-6-phenylthionicotinate having a melting point of 126°-128° C. The physical properties of this compound were identical with those of the compound obtained in Example 7.

1. customafter which the resulting mixture was subjected to reaction at room temperature for 5 hours
2. customThe organic layer was separated
3. washwashed successively with 80 ml of water and 80 ml of saturated aqueous sodium chloride solution
4. dry with materialdried over anhydrous magnesium sulfate
5. customThe solvent was removed by distillation under reduced pressure
6. customto the crystalline material thus obtained
7. filtrationafter which the crystals thus deposited were collected by filtration