HRID1927685

反应详情

EQUATION

反应方程式

HRID 1927685 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Sodium hydride (384 mg, 16 mmol) was added to a solution of 2-{4-[2-(4-iodo-1H-imidazol-2-yl)ethyl]phenyl}pyridine (5 g, 13.3 mmol) in dimethylformamide (100 mL) at 0° C. After stirring at 0° C. for 1 hr, dimethylsulfamoyl chloride (2.15 mL, 20 mmol) was added. After stirring at rt overnight, the reaction mixture was poured into water and extracted with ethyl acetate. The extracts were washed with brine, dried (sodium sulfate) and concentrated to give a residue. Chromatography of the residue over silica gel eluting with 0-20% acetone methylene chloride afforded 4-iodo-N,N-dimethyl-2-[2-(4-pyridin-2-ylphenyl)ethyl]-1H-imidazole-1-sulfonamide.

WORKUP

后处理

  1. stirringAfter stirring at rt overnight
  2. extractionextracted with ethyl acetate
  3. washThe extracts were washed with brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated
  6. customto give a residue