HRID602420

反应详情

EQUATION

反应方程式

HRID 602420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 1-(4-cyano-pyridin-2-yl)-3-methyl-urea (12.0 g, 11.4 mmol) in THF (80 mL) was treated with Raney nickel (0.5 g) placed under a hydrogen atmosphere (atmospheric pressure) for 8 hours at rt. The reaction mixture was diluted with EtOAc, filtered over Celite® and concentrated in vacuo. The residue was purified by chromatography on silica gel (Gradient elution: 100% CH2Cl2 to 85%/15% CH2Cl2/MeOH) to give 1-(4-aminomethyl-pyridin-2-yl)-3-methyl-urea (4.8 g) as a solid.

WORKUP

后处理

  1. customfor 8 hours
  2. customat rt
  3. filtrationfiltered over Celite®
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography on silica gel (Gradient elution: 100% CH2Cl2 to 85%/15% CH2Cl2/MeOH)