HRID480063

反应详情

EQUATION

反应方程式

HRID 480063 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a solution of 4-ethylbenzoic acid (3.80 g) in anhydrous acetonitrile (100 mL) was added under a nitrogen atmosphere, triphenylphosphine (20 g), 2-amino-2-methyl-1-propanol (2.74 mL) and triethylamine (28.2 mL). The mixture was cooled on an ice bath and then tetrachloromethane (5.36 mL) was added. The reaction mixture was allowed to stand at room temperature and stirred for 18 hours. To the reaction mixture was added ethyl acetate and hexane and the precipitate was removed by filtration. The concentration of the filtrate left a residue, which was purified by column chromatography on silica gel (hexane/ethyl acetate/=9/1/ to 6/1) to give the subject compound (1.15 g).

WORKUP

后处理

  1. temperatureThe mixture was cooled on an ice bath
  2. customto stand at room temperature
  3. customthe precipitate was removed by filtration
  4. waitThe concentration of the filtrate left a residue, which
  5. customwas purified by column chromatography on silica gel (hexane/ethyl acetate/=9/1/ to 6/1)