Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 22902443 | HCID 22902443 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 131720256 | HCID 131720256 | — |
Reaction Steps
1.1 g of 6,11-dihydrodibenz[b,e]oxepin-11-methanol was dissolved in 30 ml of dichloromethane, and 2.7 ml of triethylamine and 2.3 ml of 2,6-diisopropyl isocyanate were added thereto with cooling on ice. The mixture was stirred for 15 hours at room temperature, and 100 ml of water was added to the reaction mixture, and then extracted with dichloromethane. The thus obtained organic layer was washed first with 1N hydrochloric acid and then with a saturated saline solution, dried and concentrated to dryness under reduced pressure. The solid residue was purified by silica gel column chromatography (using an eluting solvent of 1/9 (v/v) ethyl acetate/toluene). The crude product was recrystallized from ethyl acetate to obtain 0.97 g of Compound 6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05679703 |
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| Source dataset | uspto-grants-1997_10 |
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| ORD ID | ord-a2db3e68c3e04f34ab7bc095f5cfa4a5 |
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| Source note | uspto-grants-1997_10 |
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