Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Iodide | HCID 5238 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | HCID 18001039 | HCID 18001039 | — |
| Reactant | HCID 22258337 | HCID 22258337 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 17830871 | HCID 17830871 | 9.8% |
Reaction Steps
To a suspension of 7-chloro-5-methoxycarbonylmethyl-1-(2-methoxy-4-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (2.6 g) in ethanol (100 ml) are added sodium carbonate (1.5 g), o-xylene dibromide (1.87 g) and sodium iodide (2.42 g), and the mixture is stirred at 60-70° C. for three hours. The mixture is evaporate to remove the solvent, and to the residue is added water, and the mixture is extracted with ethyl acetate. The extract is dried, and evaporate to remove the solvent. The residue is purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:10→1:5) to give 7-chloro-5-methoxycarbonylmethyl-1-[2-methoxy-4-(2-isoindolinyl)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.32 g) as colorless amorphous.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06335327B1 |
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| Source dataset | uspto-grants-2002_01 |
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| ORD ID | ord-6e67d07539204826931359aa4614729c |
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| Source note | uspto-grants-2002_01 |
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