HRID5943

反应详情

EQUATION

反应方程式

HRID 5943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A solution of 198 mg of 5-fluoro-3-methyl-1H-indole-2-propanoic acid in 20 ml of dry DMF is cooled at 0° C., and treated with 155 mg of 55% NaH. The reaction mixture is stirred for 60 minutes at 0° C., then 307 mg of 1-[4-(chloro-methyl)phenyl]-1H-imidazole hydrochloride are added portionwise under nitrogen at 0° C. After stirring at room temperature for 16 hours the mixture is poured into water and washed with methylene chloride. The aqueous solution is neutralized with diluted HCl and extracted with methylene chloride. The organic layer is dried over sodium sulfate and evaporated to dryness. The residue, taken up with acetone, filtered and dried, yields 35 mg of the title compound (m.p. 222° C.)

WORKUP

后处理

  1. stirringAfter stirring at room temperature for 16 hours the mixture
  2. washwashed with methylene chloride
  3. extractionextracted with methylene chloride
  4. dry with materialThe organic layer is dried over sodium sulfate
  5. customevaporated to dryness
  6. filtrationfiltered
  7. customdried