HRID59063
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 solution of 2,6-dichloro-5-methylpyrimidine-4-carbaldehyde (0.325 g, 1.70 mmol) in ethanol (10 mL) sodium borohydride (0.032 g, 0.85 mmol) was added at 0° C. The mixture was stirred for 10 minutes. Acetic acid (4 drops) was added and the volatiles were removed in vacuum. The residue was treated with 10% solution of methanol in chloroform (10 mL). The slurry was filtered through a pad of silica gel. The filtrate was concentrated and purified by column chromatography on silica using a gradient 0-4% of methanol in dichloromethane as eluent to yield the title product, 0.23 g (71%).
WORKUP
后处理
- customthe volatiles were removed in vacuum
- additionThe residue was treated with 10% solution of methanol in chloroform (10 mL)
- filtrationThe slurry was filtered through a pad of silica gel
- concentrationThe filtrate was concentrated
- custompurified by column chromatography on silica using a gradient 0-4% of methanol in dichloromethane as eluent