HRID349545

反应详情

EQUATION

反应方程式

HRID 349545 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was refluxed for 7 days
  2. temperatureAfter cooling on an ice bath
  3. customThe insoluble materials were removed by filtration
  4. additionTo the filtrate was added ethyl formate
  5. temperaturethe mixture was refluxed for 24 hours
  6. customAfter evaporation of the solvent in vacuo
  7. customthe residue was triturated with diisopropyl ether
  8. customdried in vacuo