2,3-Difluorobenzoic acid synthesis
- Product Name:2,3-Difluorobenzoic acid
- CAS Number:4519-39-5
- Molecular formula:C7H4F2O2
- Molecular Weight:158.1
Yield:4519-39-5 91%
Reaction Conditions:
at -65 - -60; for 6 h;Temperature;
Steps:
6.B (B) Addition reaction:
General procedure: Temperature control -65 ~ -60 ° C,Passing carbon dioxide into the reaction solution containing lithium 2,3-difluorobenzene,The molar ratio of carbon dioxide to metal substitution reagent is 1.5:1,The incubation time was 4 hours.Add water to hydrolyze,The mass ratio of the added water to the reaction liquid containing lithium 2,3-difluorobenzene is 1.5:1.The hydrolysis temperature is 15 to 20 °C.The organic solvent is then separated by heat distillation and concentrated and recovered.The temperature is controlled at 20 to 22 ° C and acidified with 10% hydrochloric acid.The molar ratio of acid to metal-substituted reagent is 2:1.After the addition of the hydrochloric acid solution, the reaction was kept for 3 hours. Cool down to 0 ° C,The crystal obtained by suction filtration was washed with a buffer solution of pH=2.Then wash,Dry to obtain 2,3-difluorobenzoic acid.The product obtained has a purity of 99.5% and a product yield of 90%.
References:
CN108658759,2018,A Location in patent:Paragraph 0032; 0037
124-38-9
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