Salicylic acid synthesis
- Product Name:Salicylic acid
- CAS Number:69-72-7
- Molecular formula:C7H6O3
- Molecular Weight:138.12
88-65-3
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69-72-7
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Yield:69-72-7 98%
Reaction Conditions:
Stage #1: 2-bromobenzoic-acidwith water;sodium carbonate for 1 h;Heating / reflux;
Stage #2: with water;trans-N,N'-dimethyl-1,2-cyclohexyldiamine;copper(ll) bromide at 80; for 1 h;
Stage #3: with hydrogenchloride in water at 25;Product distribution / selectivity;
Steps:
1
Under nitrogen, 2.00 g (9.95 mmol) of 2-bromobenzoic acid was combined with 10 g of H2O. 1.11 g (10.45 mmol) of Na2CO3 was then added. The mixture was heated to reflux with stirring for 30 min, remaining under a nitrogen atmosphere. Another 1.58 g (14.92 mmol) of Na2CO3 was added to the reaction mixture and reflux was continued for 30 min. Separately, 22 mg of CuBr2 and 28 mg of rac-trans-N,N'-dimethylcyclohexane-1,2-diamine (Ligand F) were combined with 2 mL H2O under nitrogen to give a deep purple solution. This solution was added to the stirred reaction mixture via syringe at 80° C. under nitrogen and stirred for 1 h at 80° C. After cooling to 25° C., the reaction mixture was acidified with 15% HCl, producing a white precipitate. The white precipitate was filtered and washed with water. After drying, a total of 1.34 g (9.7 mmol, 98% yield) salicylic acid was collected. The purity was determined by 1H NMR to be about 99%.
References:
US7335791,2008,B1 Location in patent:Page/Page column 18
90-01-7
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69-72-7
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606-45-1
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69-72-7
1320 suppliers
$5.00/10g