HRID280095

反应详情

EQUATION

反应方程式

HRID 280095 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

2.25 g 2-Chloroquinazoline, 4.2 g 1-(3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl)piperazine and 2 ml triethylamine in 8 ml isopropanol are stirred and heated 21/2 hours at 80° C. The solvent is then evaporated in vacuo and the residue is taken up in hexane. The hexane solution is treated with charcoal, filtered and concentrated whereby the ketal of the title compound crystallizes out. The resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid. After 1 hour the acidic solution is made alkaline with aqueous ammonia. The resulting precipitate is filtered off and recrystallized from ethyl acetate to give the title compound, m.p. 129°-131° C.

WORKUP

后处理

  1. customThe solvent is then evaporated in vacuo
  2. additionThe hexane solution is treated with charcoal
  3. filtrationfiltered
  4. concentrationconcentrated whereby the ketal of the title compound
  5. customcrystallizes out
  6. dissolutionThe resulting precipitate is dissolved in 40 ml aqueous 1N hydrochloric acid
  7. filtrationThe resulting precipitate is filtered off
  8. customrecrystallized from ethyl acetate