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
To a suspension of 8.2 g (0.2 mole) of lithium aluminum hydride in 150 ml of dry tetrahydrofuran was added portionwise, 18.3 g (70.0 mmole) of solid 5-oxo-1-(phenylmethyl)-N-(2-propyl)-3-pyrrolidinecarboxamide. When the addition was complete, the reaction mixture was stirred at room temperature for 18 hours and then refluxed for two hours. After cooling to room temperature, the mixture was treated dropwise, successively, with 8 ml of water, 8 ml of 15% aqueous sodium hydroxide and 24 ml of water, titrating the final addition to produce a granular precipitate. The solid was removed by filtration, washed with tetrahydrofuran and the filtrate evaporated in vacuo to give 15.6 g of 1-(phenyl-methyl)-N-(2-propyl)-3-pyrrolidinemethanamine as a heavy syrup.
WORKUP
后处理
- additionwas added portionwise
- additionWhen the addition
- temperaturerefluxed for two hours
- temperatureAfter cooling to room temperature
- additionthe mixture was treated dropwise
- additionaddition
- customto produce a granular precipitate
- customThe solid was removed by filtration
- washwashed with tetrahydrofuran
- customthe filtrate evaporated in vacuo