HRID2255038

反应详情

EQUATION

反应方程式

HRID 2255038 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 13,8 of 2,4-diallylamino-6-(piperazin-1-yl)-1,3,5-triazine [of which the hydrochloride melts (K) at 259°-263° C.] and 12.6 g of 5-chloro-10,11-dihydro-5H-dibenzo[a,d]cycloheptene [melting (K) at 110° C.] in 200 ml of toluene, 20 ml of dimethylformamide and 5.56 g of triethylamine are heated at reflux for 8 hours. When the reaction is complete, the solution is treated with 50 ml of water, and the toluene layer is decanted off. This operation is carried out a further two times. The toluene phases are combined and the toluene is evaporated. The oily residue (26 g) is dissolved at the boil in 150 ml of ethanol. The product crystallises. 10 g of 2,4-diallylamino-6-{4-(10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazin-1-yl}-1,3,5-triazine crystals, m.p. (K): 192° C., are isolated.

WORKUP

后处理

  1. customat 259°-263° C.
  2. temperatureare heated
  3. temperatureat reflux for 8 hours
  4. customthe toluene layer is decanted off
  5. customthe toluene is evaporated
  6. dissolutionThe oily residue (26 g) is dissolved at the boil in 150 ml of ethanol
  7. customThe product crystallises