反应详情

The solution of 4-chloro-2-(hydroxymethyl)thiophenol (1.0 g) from Example 16, 5-fluoro-N-methyl-2-nitroaniline (1.0 g) and K2CO3 (0.81 g) in DMF (20 ml) was heated at 90° C. for 15 minutes. After leaving the solution to stand at room temperature, water was added to the solution prior to extraction in ethyl acetate. The organic layer was washed with saturated sodium chloride solution, and dried over anhydrous sodium sulfate. After removal of the solvent under reduced pressure, the residue was purified by chromatography on a silica gel column (methylene chloride) to give the title compound (1.62 g; 85%).

1. customAfter leaving the solution
2. customto stand at room temperature
3. extractionto extraction in ethyl acetate
4. washThe organic layer was washed with saturated sodium chloride solution
5. dry with materialdried over anhydrous sodium sulfate
6. customAfter removal of the solvent under reduced pressure
7. customthe residue was purified by chromatography on a silica gel column (methylene chloride)