1-(Difluoromethyl)-3-nitro-benzene synthesis
- Product Name:1-(Difluoromethyl)-3-nitro-benzene
- CAS Number:403-25-8
- Molecular formula:C7H5F2NO2
- Molecular Weight:173.12
99-61-6
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Yield:403-25-8 99%
Reaction Conditions:
with diethylamino-sulfur trifluoride in dichloromethane at -78 - 20;
Steps:
28.1
Step 1 : DAST (16.5 mL, 125 mmol) was added dropwise to a -78 °C solution of 3- nitrobenzaldehyde (3.78 g, 25 mmol) in dichloromethane (20 mL). The mixture was stirred for 15 min and then allowed to warm to room temperature. After 4 hrs, TLC showed incomplete conversion, so the mixture was cooled again to -78 °C and additional DAST (1 .5 mL, 125 mmol) was added. The mixture was allowed to warm to room temperature and was stirred overnight. The mixture was poured in ice and dilute NH40H(aq) and extracted 2x with dichloromethane. The combined organic extracts were washed with brine and dried over sodium sulfate. Filtration and solvent evaporation gave a residue which was passed over a short plug of silica eluting with 10% ethyl acetate in hexanes to yield 1 -(difluoromethyl)-3-nitrobenzene (4.3 g, 24.8 mmol, 99%).
References:
WO2011/75515,2011,A1 Location in patent:Page/Page column 262
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![Benzene, [2,2-difluoro-1-[(trimethylsilyl)oxy]ethenyl]-](/CAS/20200611/GIF/86340-78-5.gif)
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