Hydrochloric Acid → HCID 21530375, compound

HRID 1657827Notes

Reaction equation

HRID 1657827 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]1

Participants

4

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

  1. customA heavy oil separated
  2. distillationThe solvent was distilled under reduced pressure and acetone
  3. additionwas added to the residue
  4. temperatureThe resulting mixture was heated on a steam-bath until the residue
  5. customhad crystallized
  6. temperatureThe mixture was cooled
  7. filtrationfiltered
  8. 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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