HRID1156887

反应详情

EQUATION

反应方程式

HRID 1156887 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-hydroxymethylphenyl)ethane (10.2 g) was dissolved in 40 ml of pyridine, and with stirring under ice cooling, 25 g of 4-nitrobenzoyl chloride was added gradually. The mixture was stirred at room temperature for 4 hours and then at 50° C. for 1 hour, and poured into ice water. The crystals precipitated were washed in water, dried, and recrystallized from tetrahydrofuran-benzene to afford 24.3 g of 1-(4-nitrobenzoyl)-amino-2-[2-(4-nitrobenzoyloxymethyl)phenyl]ethane having a melting point of 168.2° to 169.7° C.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature for 4 hours
  2. customThe crystals precipitated
  3. washwere washed in water
  4. customdried
  5. customrecrystallized from tetrahydrofuran-benzene