Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Potassium | HCID 5462222 | — |
| Reactant | HCID 69019215 | HCID 69019215 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 10278294 | HCID 10278294 | 11% |
Reaction Steps
2-methyl, 2-propanol, potassium salt (0.044 mol) was added to a mixture of intermediate (2) (0.011 mol) in 2-propanol (160 ml). The mixture was stirred for 48 hours, hydrolized and extracted with DCM and methanol. The organic layer was separated, dried (MgSO4), filtered and the solvent was evaporated till dryness. The residue (4.1 g) was purified by column chromatography over silica gel (eluent: toluene/2-propanol/NH4OH 90/10/1 and 85/15/1; 15–40 μm). The pure fractions were collected and the solvent was evaporated. The residue was crystallized from 2-propanone and diethyl ether. The precipitate was filtered off and dried, yielding 0.58 g (11%) of 5-(3-chlorophenyl)-7-[(4-chlorophenyl)hydroxy(1-methyl-1H-imidazol-5-yl)methyl]-1,5-dihydro-4,1-benzoxazepin-2(3H)-one, mp. 260° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07153958B2 |
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| Source dataset | uspto-grants-2006_12 |
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| ORD ID | ord-9733b6fe4044484ba09141af6860c22e |
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| Source note | uspto-grants-2006_12 |
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