Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 20572540 | HCID 20572540 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 20572512 | HCID 20572512 | 75% |
Reaction Steps
A solution of 2.3 g (0.00457 mole) of 6-chloro-7,8-methylenedioxy-1-(p-N,N-dimethylsulfamylphenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine trifluoroacetamide, 75 ml of methanol and 0.5 g of sodium hydroxide was stirred at room temperature for 2 hours, diluted with water and extracted several times with ethyl acetate. The extracts were washed with brine, dried and concentrated. The crude residue was chromatographed on 75 g of silica gel with a gradient of 1% to 4% of methanol in chloroform. The homogeneous cuts were combined and concentrated to give 1.4 g (75%) of 6-chloro-7,8-methylenedioxy-1-(p-N,N,-dimethylsulfamylphenyl)-2,3,4,5-tetrahydro-1H-3-benzazepine. A field description mass spectrogram showed an intense peak for m/e of 408 which is consistent with the structure. NMR and IR spectra also agreed with the structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04285938 |
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| Source dataset | uspto-grants-1981_08 |
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| ORD ID | ord-6b6798ef58e54c5693f0eb82e3438b86 |
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| Source note | uspto-grants-1981_08 |
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