反应详情

温度

65 °C

To a solution of 2.03 g. (7.3 millimoles) of 3-(5-tetrazolyl)dibenzo[b,f]thiepin in 100 cc. glacial acetic acid is added 15 cc. 30% aqueous hydrogen peroxide. The mixture is heated to 65° C. for 10 minutes; the sulfoxide separates from the hot solution. After cooling and diluting with water, the crystalline product is filtered and washed with water. It is then heated on a steam bath in 25 cc. DMF and filtered hot. The solid is washed with methanol and dried. The yield of sulfoxide is 1.55 g. (72%) as a white solid decomposing at 277° C.-279° C.

1. temperatureAfter cooling
2. filtrationthe crystalline product is filtered
3. washwashed with water
4. temperatureIt is then heated on a steam bath in 25 cc
5. filtrationDMF and filtered hot
6. washThe solid is washed with methanol
7. customdried
8. customat 277° C.-279° C.