HRID2368498

反应详情

EQUATION

反应方程式

HRID 2368498 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl 1-(4-fluorophenyl)-1H-imidazole-5-carboxylate (14) (5 g, 21.4 mmol), N-iodosuccinimide (12 g, 53.4 mmol), and THF (100 mL) was refluxed overnight. A solution of saturated sodium thiosulfate was added and the reaction was extracted with ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel (0-100% EtOAc in hexanes) to give ethyl 1-(4-fluorophenyl)-2-iodo-1H-imidazole-5-carboxylate (38).

WORKUP

后处理

  1. extractionthe reaction was extracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash column chromatography on silica gel (0-100% EtOAc in hexanes)