HRID1156867

反应详情

EQUATION

反应方程式

HRID 1156867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Forty (40) grams of 4-bromobenzoic acid was dissolved in 200 ml of dry dimethylformamide. While the solution was cooled with ice with stirring, 23 g of triethylamine and 22 g of ethyl chloroformate were added. After a lapse of 30 minutes, 28 g of 1-amino-2-(2-methylphenyl)ethane was added dropwise. The mixture was stirred at room temperature for 1 hour and then at 50° to 60° C. for 1 hour, and poured into ice water. The crystals precipitated were washed in water, dried, and recrystallized from cyclohexane to afford 49 g of 1-(4-bromobenzoylamino)-2-(2-methylphenyl)ethane as colorless needles having a melting point of 101.5° to 103.0° C.

WORKUP

后处理

  1. temperatureWhile the solution was cooled with ice
  2. stirringThe mixture was stirred at room temperature for 1 hour
  3. customThe crystals precipitated
  4. washwere washed in water
  5. customdried
  6. customrecrystallized from cyclohexane