HRID252992

反应详情

EQUATION

反应方程式

HRID 252992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Carbon bisulfide (4 ml) was added to a solution of 1.81 g (10 mmol) of 2-nitrobenzohydrazide in 8 ml of methanol. A solution of 616 mg (11 mmol) of potassium hydroxide in methanol (10 ml) was added thereto, and the mixture was stirred at room temperature for 6 hr. The precipitated crystal was collected by filtration and was dried. The dried crystal was added dropwise to 5 ml of concentrated sulfuric acid, and the mixture was stirred at room temperature for 3 hr. The reaction solution was added dropwise to 100 ml of ice water, and the resultant precipitate was collected by filtration and was dried to give 1.21 g (51%) of the title compound.

WORKUP

后处理

  1. filtrationThe precipitated crystal was collected by filtration
  2. customwas dried
  3. additionThe dried crystal was added dropwise to 5 ml of concentrated sulfuric acid
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. additionThe reaction solution was added dropwise to 100 ml of ice water
  6. filtrationthe resultant precipitate was collected by filtration
  7. customwas dried