Methyl 3-bromo-5-chloro-2-fluorobenzoate synthesis
- Product Name:Methyl 3-bromo-5-chloro-2-fluorobenzoate
- CAS Number:1353575-32-2
- Molecular formula:C8H5BrClFO2
- Molecular Weight:267.48
67-56-1
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Yield:1353575-32-2 91%
Reaction Conditions:
with sulfuric acidReflux;
Steps:
II.3
A solution of 3-bromo-5-chloro-2-fluorobenzoic acid (7.5 g, 29.6 mmol) in methanol (100 mL, 2470 mmol) was treated with cone. H2S04 (8 mL, 29.6 mmol) and the resulting mixture was heated to reflux overnight. The reaction mixture was allowed to cool to rt, diluted with ice water (200 mL), and extracted with EtOAc (2 X 200 mL). The combined organic extracts were washed with saturated aqueous Na2C03 solution (2 X 100 mL), brine (100 mL), dried (Na2S04), and concentrated to furnish methyl 3-bromo-5-chloro- 2-fiuorobenzoate (7.2 g, 26.9 mmol, 91 % yield) as a pale yellow solid: 1H NMR (400 MHz, CDC13) δ ppm 3.95 (s, 3 H) 7.69 - 7.77 (m, 1 H) 7.86 (dd, J=5.5, 2.4 Hz, 1H).
References:
WO2011/161216,2011,A1 Location in patent:Page/Page column 28
1996-30-1
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1269440-82-5
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