HRID1275366
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 mixture of N-(6-chloro-3-pyridylmethyl)-S-methyl-N'-nitroisothiourea (1.3 g) and acetonitrile (10 ml) was added pyridine (1.6 g) and further dropwise acetyl chloride (0.79 g) under ice-cooling. After stirring for 1 hour under ice-cooling, the mixture was warmed to room temperature and stirred at the same temperature for 2 hours. The reaction mixture was concentrated and 50 ml of ether and 5 ml of 2N hydrochloric acid were added to the mixture which was then partitioned. The resultant organic layers were dried over anhydrous magnesium sulfate and concentrated to afford 1.6 g of N-acetyl-N-(6-chloro-3-pyridylmethyl)-S-methyl-N'-nitroisothiourea as a red oil.
WORKUP
后处理
- temperaturecooling
- temperaturecooling
- stirringstirred at the same temperature for 2 hours
- concentrationThe reaction mixture was concentrated
- addition50 ml of ether and 5 ml of 2N hydrochloric acid were added to the mixture which
- customwas then partitioned
- dry with materialThe resultant organic layers were dried over anhydrous magnesium sulfate
- concentrationconcentrated