HRID979315

反应详情

EQUATION

反应方程式

HRID 979315 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 5-hydroxy-12H-benzo[a]phenothiazine-7,7-dioxide (594 mg) in THF (10 ml) was added 2,3-dichloro 5,6-dicyano-1,4-benzoquinone (1.021 gram). The mixture was stirred at room temperature for 2 minutes, then there was added n-propyl amine (0.2 ml). The stirring was continued for 0.5 hour, then the mixture was evaporated to dryness. To the residue was added 50 ml dichloromethane and the mixture was stirred for 15 minutes and filtered. The filtrate was evaporated to dryness and the residue crystallized from a mixture of toluene and hexane to afford the title compound (442 mg) as a red-brown crystalline solid, m.p. 149°-151° C. (dec.).

WORKUP

后处理

  1. waitThe stirring was continued for 0.5 hour
  2. customthe mixture was evaporated to dryness
  3. additionTo the residue was added 50 ml dichloromethane
  4. stirringthe mixture was stirred for 15 minutes
  5. filtrationfiltered
  6. customThe filtrate was evaporated to dryness
  7. customthe residue crystallized from a mixture of toluene and hexane