Hydrochloric Acid → HCID 21530375, compound
Reaction equation
[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][CH:4]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[O:10])[CH2:3]1.Cl>C(OCC)C>[ClH:17].[CH3:1][N:2]1[CH2:7][CH2:6][CH2:5][CH:4]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[Cl:17])=[O:10])[CH2:3]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
1-Methyl-3-(2-chlorophenacyl)piperidine, 24.8 g, was dissolved in 100 ml of diethyl ether. To the resulting solution was added an excess of ethereal hydrogen chloride solution. A heavy oil separated. The solvent was distilled under reduced pressure and acetone was added to the residue. The resulting mixture was heated on a steam-bath until the residue had crystallized. The mixture was cooled, filtered, and thoroughly washed with diethyl ether, giving 26.7 g of 1-methyl-3-(2-chlorophenacyl)piperidine hydrochloride, mp 136°-138°. A small portion of the salt was recrystallized from acetone to give an analytical sample, mp 135.5°-138°, from which the following elemental analysis was obtained:
Workup
- customA heavy oil separated
- distillationThe solvent was distilled under reduced pressure and acetone
- additionwas added to the residue
- temperatureThe resulting mixture was heated on a steam-bath until the residue
- customhad crystallized
- temperatureThe mixture was cooled
- filtrationfiltered
- washthoroughly washed with diethyl ether
Sources & evidence
- ORD record
- ord-d8d6ddef121144058d49f82fca3d2e84
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03962257
Reaction notes
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