反应详情

温度

-78 °C

Dibenzo[b,e][1,4]dioxine (2 g, 10.86 mmol), was taken in dichloromethane (10 ml), 2-chloroacetyl chloride (2.0 ml, 24.97 mmol) was added and the reaction was cooled to −78° C. Aluminium chloride (5.79 g, 43.4 mmol) was added carefully and was stirred for additional 2 h at −78° C., then slowly allowed to reach rt and stirred for additional 2 h. Cooled to 0° C. and ice was added, stirred for few min, white precipitation noticed, MeOH (5 mL) was added and stirred for 1 h. The precipitate was filtered and washed with water and used in the next step. Yield: 1.8, 50%; ES LC-MS m/z=337 (M−H+);

1. customto reach rt
2. stirringstirred for additional 2 h
3. temperatureCooled to 0° C.
4. additionice was added
5. stirringstirred for few min, white precipitation
6. stirringstirred for 1 h
7. filtrationThe precipitate was filtered
8. washwashed with water