HRID1445743

反应详情

EQUATION

反应方程式

HRID 1445743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
140 °C

PROCEDURE

实验过程

Formic acid (35.8 ml) was added to 4-Hydroxycoumarin (15.8 g, 97.5 mmol) and aldehyde 3 (28.9 g, 97.6 mmol). Triethylamine (43 ml) was added (exothermic) at 0° C. It was warmed to 140° C. and stirred for 4 h at this temperature. The yellow solution was cooled to rt, ethyl acetate was added, it was washed with 1 N HCl and brine, it was dried over Na2SO4 and the solvent was removed. The slightly yellow solid was recristallized from ethylacetate to yield the title compound as a white solid in 98% purity (60% yield).

WORKUP

后处理

  1. temperatureThe yellow solution was cooled to rt
  2. washit was washed with 1 N HCl and brine, it
  3. dry with materialwas dried over Na2SO4
  4. customthe solvent was removed