HRID235622

反应详情

EQUATION

反应方程式

HRID 235622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washwhereupon rinsing
  2. temperaturethe mixture is heated
  3. temperatureunder reflux under argon for 3 hours
  4. temperatureAfter cooling
  5. additionthe mixture is treated with 480 ml of water
  6. customThe precipitated crystals are removed by filtration under suction
  7. washwashed with 20 percent ethanol and water
  8. customdried
  9. customBy recrystallization from dichloromethane/methanol/ether there