Hydrochloric Acid → 153836-44-3
Reaction equation
C([N:14]1[CH2:17][CH:16]([N:18]2[CH:22]=[CH:21][N:20]=[CH:19]2)[CH2:15]1)(C1C=CC=CC=1)C1C=CC=CC=1.[ClH:23].[H][H]>CO.O.[Pd]>[ClH:23].[ClH:23].[N:18]1([CH:16]2[CH2:17][NH:14][CH2:15]2)[CH:22]=[CH:21][N:20]=[CH:19]1Participants
6
Procedure
3.20 g of 1-benzhydryl-3-(1-imidazolyl)azetidine [prepared as described in step (a) above] were dissolved in 30 ml of methanol, and 8.90 ml of a 10% w/v solution of hydrogen chloride in methanol were added to the resulting solution. 1.60 g of a 20% w/w palladium hydroxide-on-carbon catalyst were then added to the mixture, after which the mixture was hydrogenated at 50° C. for 40 minutes in an atmosphere of hydrogen. The catalyst was then removed by filtration and the filtrate was concentrated by evaporation under reduced pressure. The resulting residue was washed with diethyl ether and dried under reduced pressure, to obtain 2.03 mg of the title compound, as a powder.
Workup
- customThe catalyst was then removed by filtration
- concentrationthe filtrate was concentrated by evaporation under reduced pressure
- washThe resulting residue was washed with diethyl ether
- customdried under reduced pressure
Sources & evidence
- ORD record
- ord-4bd7c57b4e0546ef85343002ebca9ac7
- Source dataset
- uspto-grants-1999_02
- Patent number
- US05866564
Reaction notes
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