HRID19611
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 5-(3-bromo-phenyl)-6H-pyrazolo[1,5-c]pyrimidine-7-thione (compound E3)(3.73 g) in 2M aqueous NaOH (6 ml) and methanol (100 ml) methyl iodide (0.785 ml) is added at ambient temperature. After 30 min at this temperature further methyl iodide (0.785 ml) is added After 60 min the mixture is neutralized with 2M hydrochloric acid and evaporated The residue is partitioned between dichloromethane and water and the organic phase is washed twice with water. The organic phase is dried over sodium sulfate and the crude product is purified by silica gel flash chromatography. A yellow solid (1.4 g, 36%) is obtained
WORKUP
后处理
- customevaporated The residue
- customis partitioned between dichloromethane and water
- washthe organic phase is washed twice with water
- dry with materialThe organic phase is dried over sodium sulfate
- customthe crude product is purified by silica gel flash chromatography