Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 54208456 | HCID 54208456 | — |
| Reactant | 1,2,3,4,5,6-Hexahydro-3,9-dimethylazepino[4,5-b]indole | HCID 68560092 | — |
| Catalyst | Tetrabutylammonium Chloride | HCID 70681 | — |
| Product | HCID 59368496 | HCID 59368496 | 92.1% |
Reaction Steps
The title compound was prepared by following general procedure 4. 3,9-Dimethyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole (100 mg, 0.46 mmol), tetra n-butyl ammonium chloride (6 mg, 0.023 mmol), 3-chloro-5-vinylpyridine (77 mg, 0.55 mmol) were taken into 50% NaOH (3 mL). The reaction mixture was heated overnight at 110° C. The reaction mixture was extracted with ethyl acetate and organic layer was dried over Na2SO4, and concentrated under reduced pressure to obtain 150 mg of 6-(2-(5-chloropyridin-3-yl)ethyl)-3,9-dimethyl-1,2,3,4,5,6-hexahydroazepino[4,5-b]indole as the TFA salt after purification by reverse-phase chromatography (C-18, 500 mm×50 mm, Mobile Phase A=0.05% TFA in water, B=0.05% TFA in acetonitrile, Gradient: 10% B to 80% B in 30 min., injection vol. 5 mL).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08569287B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-eac56fb0dfda4243bb956e02213298e3 |
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| Source note | uspto-grants-2013_10 |
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