Ethyl 2-Fluoro-6-nitrobenzoate synthesis
- Product Name:Ethyl 2-Fluoro-6-nitrobenzoate
- CAS Number:1154426-16-0
- Molecular formula:C9H8FNO4
- Molecular Weight:213.16
Yield:1154426-16-0 35 g
Reaction Conditions:
with potassium carbonate in N,N-dimethyl-formamide at 80; for 16 h;
Steps:
257.1 Ethyl 2-fluoro-6-nitrobenzoate
To a mixture of 2-fluoro-6-nitrobenzoic acid (20 g, 108.04 mmol), K2CO3 (29.86 g, 216.09 mmol) in DMF (200 mL) was added EtI (33.70 g, 216.09 mmol, 17.28 mL). The mixture was stirred at 80 °C for 16 h, cooled to room temperature, quenched by H2O (500 mL) and extracted with EtOAc (500 mL×2). The combined organic layers were washed by brine (400 mL), dried over Na2SO4, concentrated under reduced pressure to give a residue. The residue was purified by column chromatography (SiO2, Petroleum ether/Ethyl acetate=10/1) to provide the title compound (35 g) as a yellow oil. 1H NMR (400 MHz, DMSO-d6) d 8.14-8.06 (m, 1H), 7.91-7.81 (m, 2H), 4.40 (q, J = 7.2 Hz, 2H), 1.30 (t, J = 7.2 Hz, 3H).
References:
WO2020/5935,2020,A1 Location in patent:Paragraph 01039; 01041-01043
385-02-4
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