Benzoic acid, 2,5-difluoro-4-methyl-, methyl ester synthesis
- Product Name:Benzoic acid, 2,5-difluoro-4-methyl-, methyl ester
- CAS Number:1355488-71-9
- Molecular formula:C9H8F2O2
- Molecular Weight:186.16
67-56-1
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Yield:1355488-71-9 98%
Reaction Conditions:
with sulfuric acid for 18 h;Inert atmosphere;Reflux;
Steps:
26
Preparation 26Methyl 2,5-difluoro-4-methylbenzoateTo a suspension of 4-methyl-2,5-difluorobenzoic acid (comm, 52 g, 0.3 mol) in methanol (1 .0 L) was added concentrated sulphuric acid (3 mL) with stirring and the reaction heated to reflux under nitrogen for 18 hours. The reaction was quenched with aqueous sodium bicarbonate solution (10 %, 150 mL), concentrated in vacuo and the resulting residue partitioned between EtOAc (800 mL) and water (400 mL). The organic layer was washed with water (250 mL) and brine (100 mL), dried with sodium sulphate and concentrated in vacuo to yield the title compound as a clear oil that solidified on standing (54.7 g, 98%).1H NMR (400 MHz, CDCI3): δ 2.33 (s, 3H), 3.92 (s, 3H), 6.98 (m, 1 H), 7.58 (m, 1 H).
References:
WO2012/7868,2012,A2 Location in patent:Page/Page column 86
