Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3,5-Bis(trifluoromethyl)benzoyl chloride | HCID 101856 | — |
| Reactant | HCID 86757042 | HCID 86757042 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86757041 | HCID 86757041 | 51.3% |
Reaction Steps
3,5-di(trifluoromethyl)benzoyl chloride (0.003 mol) and then triethylamine (0.0045 mol) were added dropwise to a mixture of (±)-trans-6-[1-[2-[(3,4-dichlorophenyl)-methyl]-4-piperidinyl]-4-piperidinyl]-11,12-dihydro-6H-benzimidazo[2,1-b][3]benzazepine (0.003 mol) in CH2Cl2 (25ml). The mixture was stirred at RT overnight, washed with water and separated into its layers. The organic layer was dried, filtered and the solvent was evaporated. The residue was purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 98/2 to 96/4). The pure fractions were collected and the solvent was evaporated. The residue was dried, yielding 1.23 g (51%) of (±)-trans-1-[3,5-bis(trifluoromethyl)benzoyl]-2-[(3,4-dichlorophenyl)methyl]-4-[4-(11,12-dihydro-6H-benzimidazo[2,1-b][3]benzazepin-6-yl)-1-piperidinyl]piperidine (comp. 63).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06251894B1 |
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| Source dataset | uspto-grants-2001_06 |
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| ORD ID | ord-22c187e8e3c44b1aa803cfc49c5413ef |
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| Source note | uspto-grants-2001_06 |
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