反应详情

To a mixture of 3-methoxy-5-(trifluoromethyl)benzenethiol (1.36 g) and DMF (dry) (10 mL) were added methyl 4-chloroacetoacetate (1.146 mL) and K2CO3 (1.806 g) at room temperature. The mixture was stirred at room temperature for 1 h. The mixture was poured into water at room temperature and extracted with EtOAc. The organic layer was separated, washed successively with 1N HCl and brine, dried over MgSO4 and concentrated in vacuo. The residue was purified by silica gel column chromatography (EtOAc/hexane) to give the title compound (1.120 g).

1. extractionextracted with EtOAc
2. customThe organic layer was separated
3. washwashed successively with 1N HCl and brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified by silica gel column chromatography (EtOAc/hexane)