HRID1756981

反应详情

EQUATION

反应方程式

HRID 1756981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of α-[[(2,4,6-trimethoxyphenyl)amino]-carbonyl]-benzene acetic acid (46.73 g, 0.1353 mol), and 1,1'-carbonyldiimidazole (24.7 g, 0.152 mol) in dry THF (1.0 L) was stirred at room temperature under nitrogen for 2 hours. A white solid precipitated. To the suspension was added tridecanoic acid hydrazide (30.90 g, 0.1353 mol), and the mixture was stirred at room temperature for 17 hours, then at 40° C. for 21 hours. The mixture was chilled (+5° C.) and filtered. The filtercake was washed (THF, ether, water) and dried under house vacuum/air stream; yield 54.36 g (72%); mp 175°-180° C.

WORKUP

后处理

  1. customA white solid precipitated
  2. waitat 40° C. for 21 hours
  3. temperatureThe mixture was chilled (+5° C.)
  4. filtrationfiltered
  5. washThe filtercake was washed (THF, ether, water)
  6. customdried under house vacuum/air stream