2-amino-4,6-dimethylbenzoic acid synthesis
- Product Name:2-amino-4,6-dimethylbenzoic acid
- CAS Number:90321-33-8
- Molecular formula:C9H11NO2
- Molecular Weight:165.19
49820-06-6
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Yield:90321-33-8 41.2%
Reaction Conditions:
with dihydrogen peroxide;sodium hydroxide at 70; for 0.333333 h;
Steps:
3 Step 3 : synthesis of 2-amino-4,6-dimethylbenzoic acid 74-d
H202 (123.7 g, 1200 mmol) was added to a mixture of intermediate 74-C (35.00 g,199.8 mmol) in NaOH solution (1225 mL, 0.33g/mL) at 70°C, over 5 minutes. Themixture was heated for another 15 minutes, then cooled to 15°C. Ice was added to the mixture. The resulting mixture was extracted with ethyl acetate (300 mL x 2). The pH of the solution was adjusted to 8 with addition of concentrated HC1 at 0°C and acidified to pH 6 with acetic acid. The mixture was extracted with ethyl acetate (300 mL x 2). The organic layers were combined, washed with brine, dried over Mg504 and filtered.The filtrate was concentrated to give intermediate 74-d (17 g, yield: 41.20%).
References:
WO2016/91774,2016,A1 Location in patent:Page/Page column 79; 80
108-69-0
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35162-44-8
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99-12-7
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