(4-Methoxy-3-nitro-phenyl)-acetonitrile synthesis
- Product Name:(4-Methoxy-3-nitro-phenyl)-acetonitrile
- CAS Number:56245-07-9
- Molecular formula:C9H8N2O3
- Molecular Weight:192.17
104-47-2
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Yield:56245-07-9 69%
Reaction Conditions:
with potassium nitrate;trifluoroacetic acid in acetonitrile at -10;
Steps:
15.1 Step 1: Preparation of2-(4-methoxy-3-nitrophenyl)acetonitrile
2-(4-methoxyphenyl)acetonitrile (0.20 g, 1.36 mmol) was dissolved in acetonitrile (10 mE), to which trifluoroacetic acid (0.76 mE, 5.44 mmol) was added. The temperature thereof was lowered to -10° C. Potassium nitrate (0.12 g, 1.36061 mmol) was slowly added thereto, followed by stirring. Upon completion of the reaction, a new spot was formed under the starting material, which was confirmed by TEC. Water was added thereto to terminate the reaction, followed by neutralization with potassium carbonate. The water layer was extracted twice with ethylacetate. The ethylacetate layer was washed with water and brine, dried over sodium sulfate, and concentrated under reduced pressure. Then, purification was performed by MPEC to give the target compound 2-(4-methoxy-3-nitrophenyl)ac- etonitrile (1.80 g, 9.37 mmol, yield: 69%).‘H-NMR (300 MHz, CDC13) ? 7.83 (s, 1H), 7.57 (dd, J=8.7, 2.4 Hz, 1H), 7.15 (d, J=8.7 Hz, 1H), 3.99 (s, 3H), 3.77 (s, 2H); EC/MS 192 [M+H].
References:
US2018/111905,2018,A1 Location in patent:Paragraph 0323; 0324; 0325
61010-34-2
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13435-20-6
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119-10-8
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