HRID1038294

反应详情

EQUATION

反应方程式

HRID 1038294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Compound 2 (100 grams) was dissolved in 200 ml of dry dimethylformamide (DMF) in a pressure vessel followed by addition of 30 grams of Raney Nickel catalyst. The mixture was stirred under an atmosphere of hydrogen for about 10 hours. The disappearance of the starting material using TLC confirmed the completion of reaction. The catalyst was removed by filtration. About 80% of the DMF was distilled off under high vacuum. The compound was precipitated from the residual solution by addition to methanol to give 75 grams of pure 3 as an off-white powder. m.p: 182-185° C.

WORKUP

后处理

  1. customthe completion of reaction
  2. customThe catalyst was removed by filtration
  3. distillationAbout 80% of the DMF was distilled off under high vacuum
  4. customThe compound was precipitated from the residual solution by addition to methanol