HRID1416021

反应详情

EQUATION

反应方程式

HRID 1416021 的结构方程式

PROCEDURE

实验过程

A mixture of 0.15 g (0.43 mmol)of 2-chloromethyl-5-(3,5-dichlorophenylthio)-4-isopropyl-1-methyl-1H-imidazole (28a), 1 ml of acetonitrile and 1.5 ml of a 50% methylamine aqueous solution was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, and the residue was extracted with diethyl ether. The extract was washed with water and with saturated brine and dried over potassium carbonate. The solvent was distilled off under reduced pressure, and the residue was fractionated by silica gel chromatography (ethyl acetate:methylene chloride=1:4)to obtain 0.148 g of (Compound I-78)(yield 95%). Oil.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. extractionthe residue was extracted with diethyl ether
  3. washThe extract was washed with water and with saturated brine
  4. dry with materialdried over potassium carbonate
  5. distillationThe solvent was distilled off under reduced pressure
  6. custommethylene chloride=1:4)to obtain 0.148 g of (Compound I-78)(yield 95%)