Methyl 3-fluoro-5-methylbenzoate synthesis
- Product Name:Methyl 3-fluoro-5-methylbenzoate
- CAS Number:660416-38-6
- Molecular formula:C9H9FO2
- Molecular Weight:168.16
518070-19-4
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Yield:660416-38-6 100%
Reaction Conditions:
with potassium carbonate in acetone at 65; for 1 h;
Steps:
33.1
Step 1. methyl 3-fluoro-5-methylbenzoateTo a solution of 3-fluoro-5-methylbenzoic acid (1.50 g, 9.73 mmol, Oakwood) inAcetone (40 mL) was added Potassium carbonate (1.34 g, 9.73 mmol) followed by Methyl iodide (0.73 mL, 12 mmol) . The reaction mixture was heated to 65 °C for 1 hour, heating discontinued and stirred overnight, then heating resumed at that temperature for a further 2 hours. Additional Methyl iodide (0.5 mL, 8 mmol) was added and heating was continued for 6 hours. Solids were removed by filtration and acetone was removed in vacuo. The residue was partitioned between IN NaOH and ethyl acetate. The aqueous portion was extracted with a further two portions of ethyl acetate. The combined extracts were washed with brine, then dried over sodium sulfate, decanted and concentrated. The product so obtained was used without further purification (1.64 g, 100%). 1H NMR (300 MHz, CDC13): δ 7.66-7.63 (m, 1H), 7.51 (d, 1H), 7.10-7.04 (m, 1H), 3.91 (s, 3H), 2.40 (s, 3H).
References:
WO2012/68450,2012,A1 Location in patent:Page/Page column 134
67853-03-6
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67-56-1
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929626-18-6
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929626-17-5
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