2-FLUORO-4-N-OCTYLOXYBENZOIC ACID synthesis
- Product Name:2-FLUORO-4-N-OCTYLOXYBENZOIC ACID
- CAS Number:128895-76-1
- Molecular formula:C15H21FO3
- Molecular Weight:268.32
Yield:-
Reaction Conditions:
Stage #1: 1-Bromo-3-fluoro-4-octyloxybenzenewith magnesium in tetrahydrofuran; for 1 h;Heating / reflux;
Stage #2: carbon dioxide in tetrahydrofuran at -20 - 20;
Stage #3: with hydrogenchloride;water in tetrahydrofuran at 0;
Steps:
7.Second Step
Second StepA small portion of 23.8 g of the compound (15) dissolved in 200 mL of THF was added dropwise initially, in an argon atmosphere, to 2.3 g of dried magnesium; upon checking that reflux had started, dripping of the rest continued slowly. Once dripping was over, heating under reflux continued for 1 hour. Thereafter, the reaction system was cooled to -20° C., under an argon atmosphere, and a suitable amount of crushed dry ice was added thereto, then the temperature was raised to room temperature, followed by stirring overnight. 200 mL of 3N hydrochloric acid were then added under ice cooling, the organic layer was separated, and the aqueous layer was extracted with diethyl ether. The organic layers were combined, were washed with saturated brine, and were then dried over anhydrous magnesium sulfate. After evaporating the solvent, the organic layer was recrystallized from hexane to yield 16.4 g (61.0 mmol) of 4-octyloxy-2-fluorobenzoic acid (16).
References:
US2008/58544,2008,A1 Location in patent:Page/Page column 16-17
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