HRID235622
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
A suspension of 8.74 g of 4-aminophenol in 190 ml of ethanol is added dropwise at 50° to 11.34 g of divinyl sulfone, whereupon rinsing is carried out with 50 ml of ethanol and then the mixture is heated to boiling under reflux under argon for 3 hours. After cooling, the mixture is treated with 480 ml of water and stirred for 1 hour at 0°. The precipitated crystals are removed by filtration under suction, washed with 20 percent ethanol and water and dried. By recrystallization from dichloromethane/methanol/ether there is obtained 4-(p-hydroxyphenyl)-tetrahydro-4H-1,4-thiazine 1,1-dioxide of melting point 153°-155°.
WORKUP
后处理
- washwhereupon rinsing
- temperaturethe mixture is heated
- temperatureunder reflux under argon for 3 hours
- temperatureAfter cooling
- additionthe mixture is treated with 480 ml of water
- customThe precipitated crystals are removed by filtration under suction
- washwashed with 20 percent ethanol and water
- customdried
- customBy recrystallization from dichloromethane/methanol/ether there