HRID1477697

反应详情

EQUATION

反应方程式

HRID 1477697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In argon atmosphere, to an N,N-dimethylformamide solution (5 mL) of 6-[4-(4-fluorophenyl)piperazin-1-yl]-1,3,5-triazine-2,4(1H,3H)-dione (200 mg, 0.69 mmol) synthesized in Reference Synthesis Example 18, lithium hydride (12 mg, 1.51 mmol) was added at 0° C. and the resultant mixture was stirred for 1 hour. To the mixture, 1-chloro-4-{[4-(chloromethyl)phenoxy]methyl}benzene (183 mg, 0.69 mmol) was added and the resultant mixture was stirred at 50° C. for 2 hours and at 70° C. for 3 days. After the completion of the reaction, water and ethanol were added to the reaction solution and a resultant solid was filtered to obtain a crude product of a precursor (66St) of the title compound, which was used as it was in the next reaction below.

WORKUP

后处理

  1. additionwas added at 0° C.
  2. additionwere added to the reaction solution
  3. filtrationa resultant solid was filtered