Reacción #75378

Ecuación de reacción

KOH

NaOH

4-sulfophthalic acid

→

4-Hydroxyphthalic Acid

Disolventes

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas heated for 4 hr on an oil bath
2. 2
   TemperaturaIt was then cooled such that it
3. 3
   TemperaturaWith cooling it
4. 4
   Otroevaporated to dryness in a rotary evaporator
5. 5
   Extracciónextracted in a Soxhlet
6. 6
   Otroto separate the soluble product from the insoluble inorganics
7. 7
   OtroRecrystallized from ~2 vol

Procedimiento

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.

Fuente