Sodiumdichlorofluoroacetate synthesis
- Product Name:Sodiumdichlorofluoroacetate
- CAS Number:2837-90-3
- Molecular formula:C2Cl2FNaO2
- Molecular Weight:168.9144
15128-82-2
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2837-90-3
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1111637-77-4
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Yield:1111637-77-4 74%
Reaction Conditions:
with potassium carbonate in water;N,N-dimethyl-formamide at 105; for 20 h;
Steps:
1.1 Step 1: Synthesis of 3-(difluoromethoxy)-2-nitropyridine.
To a stirred solution of 2-nitropyridin-3-ol (5 g, 35.69 mmol) and sodium 2,2-dichloro-2-fluoroacetate (8.16 g, 53.53 mmol) in N,N-dimethylmethanamide (20 mL)and water (15 mL) was added potassium carbonate (9.86 g, 71.38 mmol) slowly. The reaction mixture was heated to 105 °C for 20 h. After cooling down the reaction mixture was diluted with water (150 mL), and the mixture was extracted with ethyl acetate (3 x 50 mL). The combined organic layers were dried over sodium sulfate and concentrated to dryness in vacuo affording 3-(difluoromethoxy)-2-nitropyridine (5 g, 74%). The residue was used innext step directly without further purification. 1H NMR (400 MHz, DMSO-d6) ?: 8.48 (dd,11 = 4.4 Hz, 12 = 1.2 Hz, 1H), 8.18 (dd, 11 = 4.4 Hz, 12 = 0.8 Hz, 1H), 7.95 - 7.91 (m, 1H),7.45 (t, I = 72.0 Hz, 1H).
References:
WO2015/91889,2015,A1 Location in patent:Page/Page column 73
