HCID 86757040, compound → HCID 86757039, compound

Participants

Reaction Steps

A mixture of (±)-cis-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[4-[5,6-dihydro-3-(hydroxymethyl)-11H-imidazo[2,1-b][3]benzazepin-11-ylidene]-1-piperidinyl]-2-(phenylmethyl)piperidine (4.5 g) and manganese dioxide (20 g) in CHCl3 (200 ml) was stirred and refluxed for 1 hour. The mixture was filtered warm over dicalite and the filtrate was evaporated. The residue as purified over silica gel on a glass filter (eluent: CH2Cl2/CH3OH 95/5). The pure fractions were collected and the solvent was evaporated. The residue was purified by HPLC (eluent: CH2Cl2/CH3OH 100/0 to 95/5). The pure fractions were collected and the solvent was evaporated, yielding 3.1 g (70%) of (±)-cis-1-[3,5-bis(trifluoromethyl)benzoyl]-4-[4-(3-formyl-5,6-dihydro-11H-imidazo[2,1-b][3]benzazepin-11-ylidene)-1-piperidinyl]-2-(phenylmethyl)piperidine (comp. 11; mp. 125.8° C.).

Provenance & Evidence