HRID251797
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
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
- filtrationThe precipitated crystal was collected by filtration
- customwas dried
- additionThe dried crystal was then added dropwise to concentrated sulfuric acid (5 ml)
- stirringthe mixture was stirred at room temperature for 3 hr
- additionThe reaction solution was added dropwise to 100 ml of iced water
- filtrationThe resultant precipitate was collected by filtration
- customwas dried