反应详情

A solution of thiochroman-4-one (9 g) in ether (27 ml) was added slowly to a mixture of lithium aluminium hydride (0.53 g) in ether (54 ml). After the end of the addition, the mixture was refluxed for 2 hours. The reaction mixture was cooled and ice was added, followed by water and by a solution of 20% H2SO4. The water phase was washed twice with ether. The ether phase was washed twice with NaOH 2N, and once with water, dried over MgSO4 and evaporated. The clear oil (8.9 g) crystallised after few hours. Rdt=97%

1. additionAfter the end of the addition
2. temperaturethe mixture was refluxed for 2 hours
3. temperatureThe reaction mixture was cooled
4. additionice was added
5. washThe water phase was washed twice with ether
6. washThe ether phase was washed twice with NaOH 2N
7. dry with materialonce with water, dried over MgSO4
8. customevaporated
9. customThe clear oil (8.9 g) crystallised after few hours