反应详情

To a solution of 5,6-dihydrothieno[2,3-b]thiopyran-4-one (5.0 g, 29.4 mmol) in ethanol (98 ml) was added a solution of hydroxylamine hydrochloride (4.9 g, 70.6 mmol) in 2:1 water-ethanol (27 ml). Sodium acetate.3H2O (9.6 g, 70.6 mmol) in 2:1 water-ethanol (27 ml) was added and the solution was heated at reflux for 2 hours. The reaction mixture was concentrated to dryness, water was added and the solid product (5.3 g, 98%) was collected and dried. An analytical sample was prepared by recrystallization from acetonitrile; m.p. 123°-124° C.

1. temperaturethe solution was heated
2. temperatureat reflux for 2 hours
3. concentrationThe reaction mixture was concentrated to dryness, water
4. additionwas added
5. customthe solid product (5.3 g, 98%) was collected
6. customdried
7. customAn analytical sample was prepared by recrystallization from acetonitrile