HRID1941287

反应详情

EQUATION

反应方程式

HRID 1941287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

1-(4-cyanobenzyl)-imidazole (1 g, 0.0054 mol) is dissolved into dry tetrahydrofuran (30 ml) and cooled to -70° C. n-BuLi in hexane (0.0054 mol) is added dropwise into the reaction mixture. After stirring for additional 30 min at -70° C. 3-(4-fluorophenyl)propyl bromide (1.5 g, 0,0069 mol) in THF (10 ml) is added to the mixture and stirring is continued for 2 hours. Then the mixture is allowed to warm to room temperature. Saturated aqueous ammonium chloride solution is added to the mixture, shaked and then the layers are separated. THF-phase is dried and evaporated to dryness. The residue is crystallized from isopropanol as hydrogen chloride salt. The filtrate is purified by flash chromatography.

WORKUP

后处理

  1. additionis added dropwise into the reaction mixture
  2. stirringstirring
  3. waitis continued for 2 hours
  4. temperatureto warm to room temperature
  5. customshaked and then the layers are separated
  6. dry with materialTHF-phase is dried
  7. customevaporated to dryness
  8. customThe residue is crystallized from isopropanol as hydrogen chloride salt
  9. customThe filtrate is purified by flash chromatography