5-nitro-2-methylbenzo[d][1,3]oxazin-4-one synthesis
- Product Name:5-nitro-2-methylbenzo[d][1,3]oxazin-4-one
- CAS Number:412341-84-5
- Molecular formula:C9H6N2O4
- Molecular Weight:206.15
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Yield:412341-84-5 89%
Reaction Conditions:
at 120; for 2 h;
Steps:
1.1 Step 1. Synthesis of 2-Methyl-5-nitro-4H-3, l-benzoxazin-4-one.
Step 1. Synthesis of 2-Methyl-5-nitro-4H-3, l-benzoxazin-4-one. [00300] 2-Amino-6-nitrobenzoic acid (25.0 g, 137 mmol) was mixed with acetic anhydride (50 mL, 529 mmol) and the resulting mixture was heated to 120°C by placing the reaction vessel containing this mixture in an oil bath for 2 hours, while monitoring reaction progress by HPLC. Next, the reaction mixture was cooled, and partially concentrated by evaporation under a stream of dry nitrogen. The reaction mixture was then diluted with 100 mL diethyl ether and cooled in a refrigerator overnight. The resulting crystals were filtered and rinsed with diethyl ether (50 mL) to provide the title compound (25.3 g, 123 mmol, 89%) as a tan, crystalline solid. XH NMR (400 MHz, CDC13) δ 7.91 (t, J = 8.0 Hz, 1H), 7.57 (dd, J = 7.8, 1.01 Hz, 1H), 7.53 (dd, J = 8.3, 1.0 Hz, 1H), 2.53 (s, 3H). MS (ESI+) calc. for [C9H6N204+H]+ 207.2, found 207.2.
References:
WO2014/110558,2014,A1 Location in patent:Paragraph 00300
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