HRID1422339

反应详情

EQUATION

反应方程式

HRID 1422339 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a cold (0° C.) solution of 4-iodo-5-methylimidazole (5.0 g, 24.0 mmol) and triethylamine (5.0 mL, 36.0 mmol) in CH2Cl2 (100 mL) and 1,4-dioxane (50 mL) was added trityl chloride (8.0 g, 29.0 mmol). The resultant mixture was stirred for 2 hours and quenched with ice and extracted with diethyl ether. The organic extracts were washed with sat. aq. NaHCO3, dried (K2CO3) and the solvent evaporated in vacuo. The product mixture was concentrated onto silica gel and chromatographed (Silica gel, 30-50% EtOAc in hexanes) to afford the title compound as a pale yellow powder.

WORKUP

后处理

  1. customquenched with ice
  2. extractionextracted with diethyl ether
  3. washThe organic extracts were washed with sat. aq. NaHCO3
  4. dry with materialdried (K2CO3)
  5. customthe solvent evaporated in vacuo
  6. concentrationThe product mixture was concentrated onto silica gel
  7. customchromatographed (Silica gel, 30-50% EtOAc in hexanes)