反应详情

温度

0 °C

To a bottle containing a cooled suspension of lithium aluminum hydride (44 g, 1.17 mol) in dry tetrahydrofuran (1.5 L) was added 3,4-dihydro-1,4-benzothiazepin-5(2H)-one (150 g, 0.84 mol) in portions at 0° C. After being refluxed for 18 hours, the reaction mixture was cooled to 0° C., followed by addition of water (25 mL) dropwise. The reaction mixture was then filtered through a pad of celite and washed with dichloromethane. The filtrate was dried over sodium sulfate and evaporated in vacuo to afford 125 g of 2,3,4,5-tetrahydro-1,4-benzothiazepine (yield was 90%), which was used for the next step without further purification.

1. additionTo a bottle containing
2. temperatureAfter being refluxed for 18 hours
3. filtrationThe reaction mixture was then filtered through a pad of celite
4. washwashed with dichloromethane
5. dry with materialThe filtrate was dried over sodium sulfate
6. customevaporated in vacuo