HRID1939607

反应详情

EQUATION

反应方程式

HRID 1939607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturecooling
  2. temperaturecooling
  3. stirringstirred at the same temperature for 2 hours
  4. concentrationThe reaction mixture was concentrated
  5. addition50 ml of ether and 5 ml of 2N hydrochloric acid were added to the mixture which
  6. customwas then partitioned
  7. dry with materialThe resultant organic layers were dried over anhydrous magnesium sulfate
  8. concentrationconcentrated