5-amino-2,4-difluorobenzonitrile synthesis
- Product Name:5-amino-2,4-difluorobenzonitrile
- CAS Number:952285-54-0
- Molecular formula:C7H4F2N2
- Molecular Weight:154.12
67152-20-9
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Yield:952285-54-0 83.1%
Reaction Conditions:
with iron(0);glacial acetic acid in ethanol at 20 - 50; for 4 h;Concentration;
Steps:
6.E Preparation of E.5-amino-2,4-difluorobenzonitrile
In a 250 mL single-necked flask, 2,4-difluoro-5-nitrobenzonitrile was added(17.6 g, 95.8 mmol) was dissolved in absolute ethanol (125 mL)Glacial acetic acid (34.5 g, 574.8 mmol) was added,The reduced iron powder (21.4 g, 383.2 mmol) was added in batches,Room temperature reaction 2h, 50 reaction 2h. Reaction is completed, suction filter,The filter cake was washed with ethyl acetate (20 ml x 5), the filtrate was collected,Ethyl acetate (50 ml x 5), the combined organic phases were dried over anhydrous sodium sulfate,The solvent was evaporated under reduced pressure and the residue was washed with a small amount of n-hexane (6 mL)And the filtrate was filtered to obtain 12.3 g of 5-amino-2,4-difluorobenzonitrile, the yield was 83.1%.
References:
CN106854165,2017,A Location in patent:Paragraph 0108; 0109; 0140; 0141
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