HRID894638

反应详情

EQUATION

反应方程式

HRID 894638 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 5-cyanospiro[benzo[b]furan-2(3H), 1'-cyclopropane]-3-one (185 mg.) in ethanol (10 ml.) were added dropwise 5.5 ml. of 7% aqueous solution of hydrogen peroxide and 3.7 ml. of ethanol, then, to the mixture, was added 2 N aqueous solution of sodium hydroxide to adjust pH 10 and the solution was stirred at 60° C. for 2 hours. After cooling, the reaction mixture was neutralized with diluted hydrochloric acid and diluted with ice-water. The preciptating crystals were collected by filtration, washed with water and recrystallized from ethanol to give colorless needles of 5-carbamoylspiro[benzo[b]furan-2(3H), 1'-cyclopropane]-3-one (106 mg.). m.p. 243°-244° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. filtrationThe preciptating crystals were collected by filtration
  3. washwashed with water
  4. customrecrystallized from ethanol