HRID1248363

反应详情

EQUATION

反应方程式

HRID 1248363 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1000 ml of a 1-molar solution of boron tribromide in dichloromethane are poured over 19.5 g of 5-methoxybenzocyclobutene-1-carboxylic acid methyl ester and the whole is heated at reflux for 6 hours. The whole is concentrated to dryness by evaporation and extracted by shaking with a mixture of 2000 ml of dichloromethane and 1000 ml of water and the organic phase is separated off, washed with water, dried over magnesium sulphate and concentrated to dryness by evaporation. 5-hydroxybenzocyclobutene-1-carboxylic acid methyl ester is obtained in the form of white crystals having a melting point of 108°-109° (from ether/hexane).

WORKUP

后处理

  1. temperaturethe whole is heated
  2. temperatureat reflux for 6 hours
  3. concentrationThe whole is concentrated to dryness by evaporation
  4. extractionextracted
  5. customthe organic phase is separated off
  6. washwashed with water
  7. dry with materialdried over magnesium sulphate
  8. concentrationconcentrated to dryness by evaporation