4-Methyl-2,3-dinitrophenol synthesis
- Product Name:4-Methyl-2,3-dinitrophenol
- CAS Number:68191-07-1
- Molecular formula:C7H6N2O5
- Molecular Weight:198.13
2042-14-0
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68191-07-1
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Yield:68191-07-1 39%
Reaction Conditions:
with nitric acid;acetic acid at 0 - 20; for 1 h;
Steps:
88.1 4-methyl-2,3-dinitrophenol (1):
4-methyl-2,3-dinitrophenol (1): To a solution of 4-methyl-3-nitrophenol (10 g, 65.36 mmol) in acetic acid (60 mL) was slowly added nitric acid (3.3 mL, 78.4 mmol) at 0 °C. Then the reaction mixture was stirred at room temperature for 1 h. The reaction mixture was diluted with water (10 mL) and extracted with EtOAc (3x200 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain 1 (5 g, 39%) as light yellow solid. 1H NMR (400 MHz, CDC13): 2.30 (s, 3H), 7.25 (d, J = 8.4 Hz, 1H), 7.51 (d, J = 8.4 Hz, 1H), 10.40 (s, 1H). MS m/z (M-H): 197
References:
WO2014/149164,2014,A1 Location in patent:Paragraph 00995
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