HRID1108277

反应详情

EQUATION

反应方程式

HRID 1108277 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A suspension of 2-iodo-4-(methoxycarbonyl)-1-triphenylmethylimidazole (1.978 g, 4 mmol) in 6N sodium hydroxide (15 mL) was heated at reflux for 4 hours. The resulting suspension was diluted with ethyl acetate (20 mL) and then slightly acidified with acetic acid. The resulting clear solution was extracted three times with ethyl acetate (20 mL) and the combined extracts were dried (magnesium sulfate) and concentrated in vacuo. Residual acetic acid was removed under high vacuum to give 2-iodo-1-triphenylmethylimidazole-4-carboxylic acid (1.67 g, 87%) as a white solid, mp 203-205° C.: 1H NMR (CDCl3) δ 7.60 (s, 1H), 7.38-7.20 (m, 9H), 7.18-7.09 (m, 6H).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureat reflux for 4 hours
  3. extractionThe resulting clear solution was extracted three times with ethyl acetate (20 mL)
  4. dry with materialthe combined extracts were dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. customResidual acetic acid was removed under high vacuum