HRID349545
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 (8.94 g) in tetrahydrofuran (600 ml) was added 1-propyl-5-tritylamino-1H-pyrazole-4-carbonitrile (37 g) at room temperature. The mixture was refluxed for 7 days. After cooling on an ice bath, sodium fluoride (40 g) and water (17 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. To the filtrate was added ethyl formate, and the mixture was refluxed for 24 hours. After evaporation of the solvent in vacuo, the residue was triturated with diisopropyl ether and dried in vacuo to give 4-aminomethyl-1-propyl-5-tritylaminopyrazole (30.3 g).
WORKUP
后处理
- temperatureThe mixture was refluxed for 7 days
- temperatureAfter cooling on an ice bath
- customThe insoluble materials were removed by filtration
- additionTo the filtrate was added ethyl formate
- temperaturethe mixture was refluxed for 24 hours
- customAfter evaporation of the solvent in vacuo
- customthe residue was triturated with diisopropyl ether
- customdried in vacuo