HRID544615

反应详情

EQUATION

反应方程式

HRID 544615 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4.47 g (0.015 mole) of 5-[7-(4-cyanophenoxy)heptyl]-3-methylisoxazole (Example 5), 8 ml of 30% hydrogen peroxide, 8 ml of 95% ethanol and 0.6 ml of 6 N sodium hydroxide was stirred for ten minutes. There was then added 10 ml of 95% ethanol and the reaction mixture was warmed at 40°-50° C. for 4.5 hours, then held at room temperature overnight and treated with 5% sulfuric acid to neutral pH. The mixture was cooled and the solid product collected by filtration to give 4.4 g of 5-[7-(4-carbamylphenoxy)heptyl]-3-methylisoxazole, m.p. 153°-154° C., and recrystallized from methanol.

WORKUP

后处理

  1. temperaturethe reaction mixture was warmed at 40°-50° C. for 4.5 hours
  2. temperatureThe mixture was cooled
  3. filtrationthe solid product collected by filtration