HRID1156897

反应详情

EQUATION

反应方程式

HRID 1156897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-Amino-2-(2-chlorophenyl)ethane (44.5 g) was dissolved in 140 ml of pyridine, and with stirring under cooling, 44.5 g of p-toluoyl chloride was added dropwise. The reaction was performed at room temperature for 3 hours. The reaction mixture was poured into ice water, and the crystals that precipitated were collected by filtration. The crystals were dissolved in benzene, washed successively with hydrochloric acid, water and saturated aqueous sodium chloride solution, and dried. The solvent was distilled off. The residue was recrystallized from benzene to afford 72 g of 1-(p-toluoylamino)-2-(2-chlorophenyl)ethane as colorless needles having a melting point of 106.0° to 108.5° C.

WORKUP

后处理

  1. temperatureunder cooling
  2. customthe crystals that precipitated
  3. filtrationwere collected by filtration
  4. dissolutionThe crystals were dissolved in benzene
  5. washwashed successively with hydrochloric acid, water and saturated aqueous sodium chloride solution
  6. customdried
  7. distillationThe solvent was distilled off
  8. customThe residue was recrystallized from benzene