HRID47100

反应详情

EQUATION

反应方程式

HRID 47100 的结构方程式

PROCEDURE

实验过程

In a stainless steel beaker with a steel stirrer a mixture of 300 g KOH (5.36 mole), 150 g NaOH (3.75 mole), 120 g of a 50% aqueous solution of 4-sulfophthalic acid (~0.25 mol) was heated for 4 hr on an oil bath. It was then cooled such that it remained molten and poured into 600 ml ice + water. With cooling it was neutralized to pH 9.0 without noting any precipitate of m-hydroxybenzoic acid by-product. It was then acidified, evaporated to dryness in a rotary evaporator and extracted in a Soxhlet to separate the soluble product from the insoluble inorganics. Crude yield 26 g (59%, M.P. 175°-180° C. Recrystallized from ~2 vol boiling water. Yield 19.5 g (44%), M.P. 201°-3° C.

WORKUP

后处理

  1. temperaturewas heated for 4 hr on an oil bath
  2. temperatureIt was then cooled such that it
  3. temperatureWith cooling it
  4. customevaporated to dryness in a rotary evaporator
  5. extractionextracted in a Soxhlet
  6. customto separate the soluble product from the insoluble inorganics
  7. customRecrystallized from ~2 vol