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ChemicalBook CAS DataBase List 4-Chloro-2-fluorobenzoic acid
446-30-0

4-Chloro-2-fluorobenzoic acid synthesis

3synthesis methods
-

Yield:446-30-0 89%

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;Reagent/catalyst;

Steps:

2.1; 2.2; 2.3; 2.4; 2.5; 2.6; 2.7; 2.8; 2.9; 2.10; 2.11; 2.12; 2.13; 2.14; 2.15 Example 2-2: (Also increasing the amount of initiator, catalyst, additive)

2-fluoro-4-chlorotoluene 25g (172.9mmol, 1.0eq), AIBN 1.4g (8.6mmol, 0.05eq), Co(OAc)2·4H2O 4.3g (17.3mmol, 0.1eq)NaBr 1.8g (17.3mmol, 0.1eq), dissolved in HOAc 250mL (10V), stirred for total use, the temperature of the reaction bath outside the bath was 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 25.8 g of the target product in a yield of 89%.

References:

CN110218150,2019,A Location in patent:Paragraph 0083-0113; 0138

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