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ChemicalBook CAS DataBase List 4-Trifluoromethylsalicylic acid

4-Trifluoromethylsalicylic acid synthesis

11synthesis methods
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Yield:328-90-5 86%

Reaction Conditions:

with oxygen;potassium acetate;p-benzoquinone;palladium diacetate in ISOPROPYLAMIDE at 115; under 3800.26 Torr; for 15 h;Product distribution / selectivity;

Steps:

III
III. General procedure for Pd (II) -catalyzedorfcho-hydroxylation with 5 atm 02 :A 50 mL high pressure reactor equipped with a magnetic stir bar was charged with Pd(OAc)2 (11.2 mg, 0.05 mmol), followed by the benzoic acidsubstrate (0.5 mmol), benzoquinone (54.0 mg, 0.5 mmol), KOAc (98.0 mg, 1 mmol) andN, N-dimethylacetamide (1.5 mL) . The reactor was filled with 02 (20 atm) , and then evacuated and backed-filled with 02 (5 atm, 2 times) . After the reaction mixture was stirred at 115 °C for 15 hours, it was permitted to cool to ambient temperature. The reaction was worked up and the crude product was purified following the procedure described above for hydroxylation with 1 atm O2.

References:

THE SCRIPPS RESEARCH INSTITUTE;YU, Jin-quan WO2011/37929, 2011, A2 Location in patent:Page/Page column 14; 19-20

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