HRID1823895
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Lithium aluminium hydride (1 m in THF, 10 ml, 10 mmol) was added to a solution of the amide from Step 1 (1.0 g, 4.6 mmol) in THF (20 ml) and the mixture was heated at reflux for 16 hours. The reaction was cooled in ice and treated successively with water (0.4 ml), sodium hydroxide (0.4 ml) and water (1.2 ml) allowing 10 minutes between additions. The mixture was filtered through a bed of Celite® and washed through with THF. The filtrate was evaporated in vacuo to provide 7-(N-benzylamino)hept-1-yne as a yellow oil (924 mg, 99%). (ES+) 202 ([MH]+).
WORKUP
后处理
- temperaturethe mixture was heated
- temperatureat reflux for 16 hours
- temperatureThe reaction was cooled in ice
- filtrationThe mixture was filtered through a bed of Celite®
- washwashed through with THF
- customThe filtrate was evaporated in vacuo