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ChemicalBook CAS DataBase List 5-METHOXY-2-METHYL-4-NITROBENZOIC ACID
1401423-31-1

5-METHOXY-2-METHYL-4-NITROBENZOIC ACID synthesis

2synthesis methods
5-METHOXY-2-METHYL-4-NITROBENZONITRILE

1401423-29-7
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5-METHOXY-2-METHYL-4-NITROBENZOIC ACID

1401423-31-1
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Yield:1401423-31-1 91%

Reaction Conditions:

with sulfuric acid in water;acetic acid at 120; for 10 h;

Steps:

5.2 Step2: 5-methoxy-2-methyl-4-nitrobenzoic acid

A mixture of 5-methoxy-2-methyl-4-nitrobenzonitrile (2.0 g, 10.4 mmol) in AcOH (20 mL), water (20 mL) and cone, sulfuric acid (20 mL) was heated to 120°C for 10 h. Water (100 mL) and DCM (100 mL) were added and the mixture was passed through a hydrophobic frit. The solvent was removed in vacuo to give 5-methoxy-2-methyl-4-nitrobenzoic acid (2.0 g, 91%) as an off-white solid. LCMS (lOcm ESCI Formic MeCN): [M - H]" = 210 at 3.37 min. ? NMR (400 MHz, CDCI3): δ 7.75 (s, 1H), 7.70 (s, 1H), 3.99 (s, 3H), 2.62 (s, 3H).

References:

WO2013/79494,2013,A1 Location in patent:Page/Page column 62; 63