Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Nitric Acid | HCID 944 | — |
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 131728532 | HCID 131728532 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 131728533 | HCID 131728533 | — |
Reaction Steps
Cooled sulfuric acid (1 mL) was added to a solution of compound of Example 37e (0.3 g, 0.85 mmol) in concentrated nitric acid (10 mL) at 0° C. The reaction mixture was stirred at 0° C. for 1.5 h. The reaction mixture was slowly poured in cold water (100 mL), solid obtained was filtered, washed with water till pH was neutral. Solid obtained was crystallized using ethyl acetate/pet. ether 60-80° C. to obtain the title compound. Yield: 0.31 g, (91.70%); 1H NMR (DMSO-d6, 300 MHz): δ 2.70 (s, 3H, CH3), 3.90 (s, 3H, OCH3), 5.30 (s, 2H, CH2), 8.10 (s, 1H, Ar), 8.15 (s, 1H, Ar), 8.35 (s, 1H, NH), 8.55 (s, 2H, Ar); MS: m/e (EI) 396 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07964631B2 |
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| Source dataset | uspto-grants-2011_06 |
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| ORD ID | ord-fc6a47e1f97145ba8ca647af958bf632 |
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| Source note | uspto-grants-2011_06 |
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