5-Carboxyphthalide synthesis
- Product Name:5-Carboxyphthalide
- CAS Number:4792-29-4
- Molecular formula:C9H6O4
- Molecular Weight:178.14
100-21-0
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Yield:4792-29-4 82%
Reaction Conditions:
with sulfuric acid;paraformaldehyde in water;
Steps:
2 5-Carboxyphthalid
Example 2 5-Carboxyphthalid Oleum (20-25% SO3 43 kg) is charged into a reactor. Terephthalic acid (13 Kg) and then paraformaldehyde (3.8 Kg) is added. The mixture is agitated at 138-148° C. for 41/2 hours. Water (87 L) is added and the temperature is adjusted to about 100° C. The precipitate is filtered of, washed with water and suspended in water. The pH of the suspension is adjusted to about 7 with NaOH (about 10%), activated carbon, 0.5 Kg is added, and then the mixture is filtered, the precipitate is rinsed with water. The temperature of the filtrate is adjusted to about 85° C. and the pH is adjusted to about 2 with 96% sulfuric acid. The 5-carboxyphthalide precipitated is separated by filtration washed and dried. Yield 82%.
References:
US6403813,2002,B1
82104-74-3
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