Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Dabco | HCID 9237 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 69521716 | HCID 69521716 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86591392 | HCID 86591392 | — |
Reaction Steps
CDI (0.00925 mol) was added to a mixture of (±)-4-[[4-(3-chlorophenyl)-1,2-dihydro-2-oxo-6-quinolinyl]hydroxy(1-methyl-1H-imidazol-5-yl)methyl]benzoic acid monohydrochloride monohydrate (described in Example B3) (0.00185 mol) in THF (10 ml). The mixture was stirred at 40° C. for 1 hour.1,4 diazabicyclo[2,2,2]octane (0.00185 mol) and methanol (5 ml) were added. The mixture was stirred at 40° C. for 18 hours, poured out into H2O and extracted with EtOAc. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated. The residue was crystallized from 2-propanone. The precipitate was filtered off and dried, yielding 0.44 g (48%) of (±-methyl 4-[[4-(3-chlorophenyl)-1,2-dihydro-2-oxo-6-quinolinyl]hydroxy(1-methyl-1H-imidazol-5-yl)methyl]benzoate, mp. 255° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07173040B2 |
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| Source dataset | uspto-grants-2007_02 |
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| ORD ID | ord-de395b684f4e451da7c16ff452d3c5f9 |
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| Source note | uspto-grants-2007_02 |
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