HRID251797

反应详情

EQUATION

反应方程式

HRID 251797 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 1.95 g (10 mmol) of 5-methyl-2-nitrobenzohydrazide in methanol (8 ml). A solution of 616 mg (11 mmol) of potassium hydroxide in methanol (10 ml) was then 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 then added dropwise to concentrated sulfuric acid (5 ml), and the mixture was stirred at room temperature for 3 hr. The reaction solution was added dropwise to 100 ml of iced water. The resultant precipitate was collected by filtration and was dried to give 1.28 g (yield 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 then added dropwise to concentrated sulfuric acid (5 ml)
  4. stirringthe mixture was stirred at room temperature for 3 hr
  5. additionThe reaction solution was added dropwise to 100 ml of iced water
  6. filtrationThe resultant precipitate was collected by filtration
  7. customwas dried