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4-Fluoro-N-methyl-3-nitrobenzenesulfonamide synthesis
- Product Name:4-Fluoro-N-methyl-3-nitrobenzenesulfonamide
- CAS Number:1041598-53-1
- Molecular formula:C7H7FN2O4S
- Molecular Weight:234.2
Yield:1041598-53-1 90%
Reaction Conditions:
with triethylamine in tetrahydrofuran at -35; for 1 h;
Steps:
1.b
b) 4-fluoro-/V-methyl-3-nitrobenzenesulfonamideTo a solution of 4-fluoro-3-nitrobenzenesulfonyl chloride (43 g, 179.5 mmol) in THF (500 mL) was added Et3N (150 mL, 1.08 mol). The mixture was cooled to -35 °C and ΟΗ3ΝΗ2·ΗΟΙ (14.5 g, 215.4 mmol) in water was added dropwise. After 1 h, the mixture was warmed to rt and diluted with 1 :1 water/EtOAc. The organic layer was separated and washed with sat. aq. NaHC03, then brine, dried over MgS04, filtered, and concentrated in vacuo. The crude residue was purified via flash column chromatography (20%EtOAc/petroleum ether) to afford the title compound (38 g, 90%) as a yellow solid.
References:
WO2011/149827,2011,A1 Location in patent:Page/Page column 52
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1493-27-2
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1041598-53-1
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