HRID2049105

反应详情

EQUATION

反应方程式

HRID 2049105 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10 g (0.037 mole) bis(2-hydroxy-5-chlorophenyl)-methane and 8.6 g (0.037 mole) 1,11-dichloro-3,6,9-trioxaundecane are dissolved in 100 ml n-BuOH. To this is added 6.5 g 50% aqueous sodium hydroxide. The resulting solution is heated to reflux for 15 hours, acidified with ethereal HCl, and solvent stripped in vacuo. The resulting gum is chromatographed on Neutral Alumina IV, eluting with ether/ethyl acetate. Appropriate fractions are collected, combined and recrystallized from methanol to yield 3.65 g white crystalline solid; m.p. 143.5°-144°. Yield: 23%.

WORKUP

后处理

  1. temperatureThe resulting solution is heated
  2. temperatureto reflux for 15 hours
  3. customThe resulting gum is chromatographed on Neutral Alumina IV
  4. washeluting with ether/ethyl acetate
  5. customAppropriate fractions are collected
  6. customrecrystallized from methanol