HRID19737
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
6,7-Dihydro-5H-[1]pyrindine-6-carboxylic acid amide (0.209 g, 1.28 mmol) is added portionwise to a suspension of LiAlH4 (0.204 g, 5.38 mmol) in THF (10 ml). After 5 minutes at ambient temperature, the reaction is heated to reflux for 1.5 hours and then cooled. Water (0.2 ml) is cautiously added, followed by 15% aqueous sodium hydroxide (0.2 ml), followed by further water (0.6 ml). The resultant granular precipitate is filtered and washed with EtOAc. The combined filtrate and washings are evaporated to afford C-(6,7-dihydro-5H-[1]pyrindin-6-yl)methylamine. δc 35.2 (t), 38.9 (t), 41.0 (d), 47.6 (t), 121.6 (d), 132.6 (d), 136.4 (s), 148.1 (s), 164.8 (s).
WORKUP
后处理
- temperaturethe reaction is heated
- temperatureto reflux for 1.5 hours
- temperaturecooled
- filtrationThe resultant granular precipitate is filtered
- washwashed with EtOAc
- customThe combined filtrate and washings are evaporated