Methyl 3-fluoro-6-iodo-2-Methylbenzoate synthesis
- Product Name:Methyl 3-fluoro-6-iodo-2-Methylbenzoate
- CAS Number:1262417-94-6
- Molecular formula:C9H8FIO2
- Molecular Weight:294.06
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Yield:-
Reaction Conditions:
Stage #1: 3-fluoro-6-iodo-2-methylbenzoic acidwith oxalyl dichloride;N,N-dimethyl-formamide in dichloromethane at 20; for 0.5 h;
Stage #2: methanol at 20; for 18 h;
Steps:
2 Step 2: Preparation of methyl 3-fluoro-6-iodo-2-methylbenzoate (i-lOb)
To a solution of 3-fluoro-6-iodo-2-methylbenzoic acid i-lOa (3.7 g, 13.2 mmol) in DCM (30 mL) were added oxalyl dichloride (5.0 g, 39.6 mmol) and DMF (48 mg, 0.66 mmol). The mixture was stirred at room temperature for 0.5 h, then concentrated. The residue was dissolved in methanol (40 mL) and the mixture was stirred at room temperature for 18 h. The mixture was concentrated and the residue was purified by flash chromatography (1:20EtOAc/hexanes) to give the title compound as a solid. ‘H NMR (400 MHz, CDC13) ? 7.60 (dd, J= 8.2 Hz, 5.1 Hz, 1H), 6.82 (t,J= 8.8 Hz, 1H), 3.96 (s, 3H), 2.24 (s, 3H).
References:
WO2017/75185,2017,A1 Location in patent:Paragraph 00158
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1262417-94-6
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