Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Methylbenzoyl chloride | HCID 70276 | — |
| Reactant | HCID 19607765 | HCID 19607765 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10297101 | HCID 10297101 | — |
Reaction Steps
5-Dimethylamino-1-(2-methyl-4-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (H) (1.00 g) is dissolved in dichloromethane (30 ml), and thereto is added triethylamine (0.48 ml) under ice-cooling, and further added dropwise 2-methylbenzoyl chloride (0.44 ml). The mixture is stirred at room temperature for 1 hour. The reaction solution is washed with water, and dried over magnesium sulfate. The solvent is distilled off, and the resulting residue is crystallized by adding thereto ethyl acetate. The precipitated crystal is recrystallized from dichloromethane/ethyl acetate to give 5-dimethylamino-1-[2-methyl-4-(2-methylbenzoylamino)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.92 g) as white powder, m.p. 191°-192° C. HPLC retention time: 7.5 minutes
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05753677 |
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| Source dataset | uspto-grants-1998_05 |
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| ORD ID | ord-58b53c91fc0b411881ef8513199f2a34 |
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| Source note | uspto-grants-1998_05 |
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