HRID65256

反应详情

EQUATION

反应方程式

HRID 65256 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

To a -10° C. solution of 8 g (0.064 mole) of 1-[2-(4-aminophenyl)ethyl]-1H-imidazole and 10 mL triethylamine in 200 mL of methylene chloride add 5 mL of methanesulfonyl chloride dropwise. Stir the resulting solution at -10° C. for about 30 minutes then warm to ambient temperature for about 30 minutes. Wash the reaction mixture with water. (2×100 mL). Extract with 10% aqueous sodium hydroxide (2×50 mL). The combined aqueous extracts are neutralized with ammonium chloride then extracted with methylene chloride (2×100 mL) and combined. Remove the solvent in vacuo to provide the title compound, which may be recrystallized from tetrahydrofuran.

WORKUP

后处理

  1. temperaturethen warm to ambient temperature for about 30 minutes
  2. washWash the reaction mixture with water
  3. extractionExtract with 10% aqueous sodium hydroxide (2×50 mL)
  4. extractionthen extracted with methylene chloride (2×100 mL)
  5. customRemove the solvent in vacuo