Methyl 4-acetyl-3-chlorobenzoate synthesis
- Product Name:Methyl 4-acetyl-3-chlorobenzoate
- CAS Number:57542-71-9
- Molecular formula:C10H9ClO3
- Molecular Weight:212.63
Yield:57542-71-9 94%
Reaction Conditions:
with potassium carbonate in N,N-dimethyl-formamide at 20; for 1 h;
Steps:
42.1
To a solution of 4-acetyl-3-chlorobenzoic acid (synthesized by the method of Tetrahedron 1988, 44, 1631 , 700 mg, 3.52 mmol) in NN-dimethylformamide (4 mL) were added potassium carbonate (974 mg, 7.05 mmol) and iodomethane (658 μ, 10.57 mmol) at room temperature, and the mixture was stirred at room temperature for 1 hour. To the reaction solution was added water, and the mixture was extracted with ethyl acetate three times. The organic layer was combined, filtered through Phase-separator (Varian Inc.), and then concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane:ethyl acetate = 100:0→75:25) to give methyl 4-acetyl-3- chlorobenzoate (707 mg, 94%) as a pale yellow powder.APCI-MS m/z:213/215[M+H]+.
References:
WO2012/124825,2012,A1 Location in patent:Page/Page column 141
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