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ChemicalBook CAS DataBase List 4-METHYL-2-NITROBENZOIC ACID

4-METHYL-2-NITROBENZOIC ACID synthesis

10synthesis methods
-

Yield: 75%

Reaction Conditions:

with oxygen;sodium hydroxide in ethanol;water at 65; under 13501.4 Torr; for 24 h;Autoclave;Solvent;Concentration;

Steps:

2 Example 2:
1,4-dimethyl-2-nitrobenzene (907 mg, 6 mmol, 1.0 eq)Sodium hydroxide (1.8 g, 45.0 mmol, 7.5 eq)Was added to a 100 ml autoclave,10 ml of 80% (v / v) ethanol (8 ml of ethanol, 2 ml of water)After charging oxygen three times,Passing oxygen gas (pressure 1.8MPa),In the oil bath temperature control 65 for 24 hoursAfter the reaction was diluted with methanol,Neutral and PH = 2-3,The solvent was removed under reduced pressure,After adding ethyl acetate, the mixture was dried and filtered.Separated by chromatography,1,4-dimethyl-2-nitrobenzene recovered 129mg (0.85mmol),The conversion of 1,4-dimethyl-2-nitrobenzene was 86%4-methyl-2-nitrobenzoic acid was obtained811 mg (4.48 mmol) in 75% yield

References:

Zhejiang University of Technology;She Yuanbin;Li Guijie;Fang Kun CN106995374, 2017, A Location in patent:Paragraph 0031; 0032; 0033; 0034; 0035; 0036; 0037-0042

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