反应详情

To a stirred solution of 2-chloro-4-methoxyaniline (7.90 g, 50.1 mmol) in saturated aqueous sodium hydrogen carbonate (40 mL) and tetrahydrofuran (40 mL) was added thiophosgene (4.99 mL, 65.1 mmol) at room temperature. After 30 min, the reaction mixture was extracted with ethyl acetate, washed with aqueous sodium hydrogen carbonate and brine, dried over sodium sulfate, filtrated, and concentrated in vacuo. The resulting solid was washed with n-hexane to give the title compound as a pale red solid (6.85 g, 34.3 mmol, 68%).

1. extractionthe reaction mixture was extracted with ethyl acetate
2. washwashed with aqueous sodium hydrogen carbonate and brine
3. dry with materialdried over sodium sulfate
4. filtrationfiltrated
5. concentrationconcentrated in vacuo
6. washThe resulting solid was washed with n-hexane