HRID1372482
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-iodo-2-hydrazinopyridine (470 mg, 2 mmol) in dichloromethane (30 mL) was added a solution of N,N-carbonyldiimidazole (389 mg, 2.4 mmol) in 20 mL of dichloromethane. After stirring at room temperature for 2 h, the mixture was washed sequentially with water, 0.5N aqueous hydrochloric acid and saturated aqueous sodium bicarbonate solution. The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure to afford the product. The resultant yellow crystals that precipitated from the aqueous phase upon standing overnight were collected and dried in vacuo to afford additional product. LC/MS 261.8 (M+1).
WORKUP
后处理
- washthe mixture was washed sequentially with water, 0.5N aqueous hydrochloric acid and saturated aqueous sodium bicarbonate solution
- dry with materialThe organic phase was dried (magnesium sulfate)
- concentrationconcentrated under reduced pressure
- customto afford the product
- customThe resultant yellow crystals that precipitated from the aqueous phase
- waitupon standing overnight
- customwere collected
- customdried in vacuo
- customto afford additional product