Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ammonia | HCID 222 | — |
| Reactant | Hydrogen Bromide | HCID 260 | — |
| Reactant | HCID 7148512 | HCID 7148512 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 69462384 | HCID 69462384 | 45% |
Reaction Steps
To 400 mg (1.55 mmol) of (2-amino-4,5-dimethoxyphenyl)(phenyl)methanone (XXIaa), add dropwise 2.1 ml of HBr 40% by weight in water. Heat at 95° C. for 12 hours. At 0° C. add ammonia to pH=8.9. Add 100 ml H2O and extract three times with 100 ml of CH2Cl2. Dry on MgSO4, evaporate the CH2Cl2 and purify by silica chromatography (AcOEt 1/hexane 4 then 1/1). Yield: 45%. 1H-NMR (CDCl3, 200 MHz): d 3.92 (s, 3H, OCH3), 6.20 (s, 1H Ar), 7.00 (s, 1H Ar), 7.42–7.61 (m, 5H Ar).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07250410B2 |
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| Source dataset | uspto-grants-2007_07 |
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| ORD ID | ord-9f1340f377034ddc9e9a7dd89553a92a |
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| Source note | uspto-grants-2007_07 |
|---|