反应详情

The product of Stage (ii) (7.28 g), potassium carbonate (9.90 g), acetone (70 ml), and dimethylsulphate (5.1 ml) were vigorously stirred at room temperature overnight under nitrogen. The mixture was concentrated to one half of its volume and then stirred with water (350 ml) for 30 min. The mixture was filtered off, washed with water (50 ml), air-dried for 1 h, and dried in vacuo over phosphorus pentoxide to give the title compound as needles (7.59 g), m.p. 157.5°-158.5°.

1. concentrationThe mixture was concentrated to one half of its volume
2. filtrationThe mixture was filtered off
3. washwashed with water (50 ml)
4. customair-dried for 1 h
5. dry with materialdried in vacuo over phosphorus pentoxide