HRID602420
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
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
- customfor 8 hours
- customat rt
- filtrationfiltered over Celite®
- concentrationconcentrated in vacuo
- customThe residue was purified by chromatography on silica gel (Gradient elution: 100% CH2Cl2 to 85%/15% CH2Cl2/MeOH)