3-Hydroxy-2,4,5-trifluorobenzoic acid synthesis
- Product Name:3-Hydroxy-2,4,5-trifluorobenzoic acid
- CAS Number:116751-24-7
- Molecular formula:C7H3F3O3
- Molecular Weight:192.09
652-03-9
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Yield:116751-24-7 90.35%
Reaction Conditions:
Stage #1: 3,4,5,6-tetrafluorophthalic acidwith sodium hydroxide in water at 90; for 9 h;
Stage #2: with hydrogenchloride;tri-n-propylamine in water at 140; pH=1; under 7500.75 Torr; for 7 h;Temperature;
Steps:
1-9 Example 5: Preparation of 2,4,5-trifluoro-3-hydroxybenzoic acid
Weigh 47.60g of tetrafluorophthalic acid and dissolve 160.0g of sodium hydroxide in 800g of distilled water into a 1500ml three-necked flask. The temperature is raised to 90°C and the reaction is stirred for 9h.Stop the reaction. Add 30.00g of tripropylamine, then add concentrated hydrochloric acid to adjust to pH=1.0, heat up to 140°C, 1Mpa stirring for 7hStop the reaction, cool to room temperature, add ethyl acetate for extraction three times, combine the organic phases, distill under reduced pressure (40°C-0.08Mpa) to recover ethyl acetate. After recovery, vacuum dry for 4 hours.36.30 g of light brown solid 2,4,5-trifluoro-3-hydroxybenzoic acid with a purity of 95.59%.The yield was 90.35%.
References:
CN111253241,2020,A Location in patent:Paragraph 0034; 0045; 0046; 0049-0064
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