4-Bromo-2-fluorobenzoic acid synthesis
- Product Name:4-Bromo-2-fluorobenzoic acid
- CAS Number:112704-79-7
- Molecular formula:C7H4BrFO2
- Molecular Weight:219.01
51436-99-8
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112704-79-7
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Yield:112704-79-7 88%
Reaction Conditions:
with 2,2'-azobis(isobutyronitrile);oxygen;cobalt(II) diacetate tetrahydrate;acetic acid;sodium bromide at 130; under 9000.9 Torr; for 1.5 h;Green chemistry;
Steps:
2-16 Example 2-16: Substrate Expansion 1
2-fluoro-4-bromotoluene 25g (132.3mmol, 1.0eq), AIBN 521mg (3.2mmol, 0.024eq),Co(OAc)2·4H2O 1.6g (6.5mmol, 0.049eq), NaBr 449mg (4.4mmol, 0.033eq), dissolved in HOAc 250mL (10V), stirred for total use, the temperature of the reaction coil outside the bath is raised To 130 ° C,The coil pressure was adjusted to 1.2 MPa with oxygen, and the batching was started. The residence time of the system was 1.5 h and the oxygen was 3 to 5 eq.The system was directly pumped into 375 mL of purified water, the pH of the system was adjusted to 12-14 with NaOH solids, and the aqueous phase was extracted twice with 125 mL of MTBE.The aqueous phase was adjusted to pH 1 with concentrated HCl, and a large amount of solid precipitated.Filtration gave the target product 25.5 g, yield 88%.
References:
CN110218150,2019,A Location in patent:Paragraph 0114-0116; 0138
625446-22-2
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124-38-9
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57848-46-1
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112704-79-7
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