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, and 37.7 g of 2-(2,4-di-t-amylphenoxy)butanoyl chloride was added thereto dropwise under refluxing. After stirring while refluxing for 1 hour, the reaction mixture was cooled to room temperature, and the crystals thus formed were collected by filtration, washed with acetonitrile, and dried to obtain crystals weighing 49.5 g. A mixture of 49 g of the resulting crystals, 28 g of reduced iron, 2.7 g of ammonium chloride, 50 ml of water, and 500 ml of isopropanol was stirred while refluxing for 1 hour. The iron powder was removed by filtration, and the filtrate was cooled to precipitate crystals, which were then collected by filtration and dried to provide 42.4 g of the desired compound.
WORKUP
后处理
- temperaturedropwise under refluxing
- temperaturewhile refluxing for 1 hour
- customthe crystals thus formed
- filtrationwere collected by filtration
- washwashed with acetonitrile
- customdried
- customto obtain crystals
- stirringwas stirred
- temperaturewhile refluxing for 1 hour
- customThe iron powder was removed by filtration
- temperaturethe filtrate was cooled
- customto precipitate crystals, which
- filtrationwere then collected by filtration
- customdried