HRID349533
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 lithium aluminum hydride (4.89 g, 129 mmol) in tetrahydrofuran (318 ml) was added 5-amino-1-[2-(trityloxy)ethyl]pyrazole-4-carbonitrile (25.4 g, 64.4 mmol) at room temperature. The mixture was stirred under reflux for 12 hours. After cooling on an ice bath, sodium fluoride (25.4 g), tetrahydrofuran (100 ml), dichloromethane (200 ml) and water (10 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. The filtrate was concentrated in vacuo to give {5-amino-1-[2-(trityloxy)ethyl]pyrazol-4-yl}methylamine (19.8 g) as a solid.
WORKUP
后处理
- temperatureunder reflux for 12 hours
- temperatureAfter cooling on an ice bath
- customThe insoluble materials were removed by filtration
- concentrationThe filtrate was concentrated in vacuo