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
20 g of 2-amino-4-chloro-5-nitrophenol was dispersed in 150 ml of acetonitrile to which 37.7 g of 2-(2,4-di-tert-amylphenoxy)butanoyl chloride was added dropwise under refluxing. After refluxing for 4 hours, the reaction mixture was cooled to deposit crystals. The crystals were collected by filtration, washed with acetonitrile and dried to yield 49.5 g thereof. 49 g of the crystals were refluxed with stirring for 1 hour together with 28 g of reduced iron powder, 2.7 g of ammonium chloride, 50 ml of water and 500 ml of isopropanol. After removing the iron powder by filtration, the filtrate was cooled to deposite the crystals. The crystals were collected by filtration and dried to obtain 42.4 g of the above described compound.
WORKUP
后处理
- additionwas added dropwise
- temperatureunder refluxing
- temperatureAfter refluxing for 4 hours
- temperaturethe reaction mixture was cooled
- filtrationThe crystals were collected by filtration
- washwashed with acetonitrile
- customdried
- customto yield 49.5 g
- customAfter removing the iron powder
- filtrationby filtration
- temperaturethe filtrate was cooled
- filtrationThe crystals were collected by filtration
- customdried
- customto obtain 42.4 g of the