4-Sulfophthalic acid → 4-Hydroxyphthalic acid

HRID 47100

반응식

HRID 47100 반응식
[OH-:1].[K+].[OH-].[Na+].S([C:9]1[CH:10]=[C:11]([C:18]([OH:20])=[O:19])[C:12](=[CH:16][CH:17]=1)[C:13]([OH:15])=[O:14])(O)(=O)=O>>[OH:1][C:9]1[CH:10]=[C:11]([C:18]([OH:20])=[O:19])[C:12](=[CH:16][CH:17]=1)[C:13]([OH:15])=[O:14]

참가 물질

4

반응물 3

HCID 69624-Sulfophthalic acidHCID 14797Potassium HydroxideHCID 14798Sodium Hydroxide

생성물 1

HCID 118814-Hydroxyphthalic acid

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8bb11f0546e44605ad5ed56446ee239b
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04176223

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