Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Cyclohexene | HCID 8079 | — |
| Reactant | 1,2,3,4-Tetrahydro-benzo(b)azepin-5-one | HCID 294788 | — |
| Reactant | Cyclopropanecarboxylic Acid 4-(1-benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulene-6-carbonyl)-2-methyl-benzylamide | HCID 57555290 | — |
| Reactant | HCID 178516958 | HCID 178516958 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178432324 | HCID 178432324 | 53% |
Reaction Steps
Cyclopropanecarboxylic acid 4-(1-benzyl-2-methyl-4,5-dihydro-1H-1,3,6-triaza-benzo[e]azulene-6-carbonyl)-2-methyl-benzylamide from Example E123.1 (155 mg, 0.31 mmol) was dissolved in absolute ethanol (10 ml) and placed under an inert atmosphere. 10% Palladium on car-bon (155 mg) and cyclohexene (0.311 ml, 3.1 mmol) were added and the mixture was heated at 60° C. for 18 h. The catalyst was filtered off through Celite® filter agent and the filtrate was concentrated in vacuo. The residue was purified by preparative HPLC (eluant; 0.5% 35% ammonia:9.5% methanol:90% dichloromethane) to give a white solid identified as the title compound (67 mg, 53%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08202858B2 |
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| Source dataset | uspto-grants-2012_06 |
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| ORD ID | ord-83e7110de6ec492681a1c858c0ede47f |
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| Source note | uspto-grants-2012_06 |
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