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Triethylamine → 1-(4'-Chloro benzyl)-2-phenyl-4-(piperidino ethyl) piperazine

HRID 1581001
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Reaktionsgleichung

Reaktionsgleichung von HRID 1581001
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][NH:10][CH2:9][CH:8]2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1.[N:21]1([CH2:27][CH2:28]Cl)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1.C(N(CC)CC)C>CC(C)=O>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([CH2:6][N:7]2[CH2:12][CH2:11][N:10]([CH2:28][CH2:27][N:21]3[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]3)[CH2:9][CH:8]2[C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[CH:4][CH:3]=1
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Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 748271-(2-Chloroethyl)piperidineHCID 214485281-(4'-Chloro benzyl)-2-phenyl piperazine

Produkt 1

HCID 537184121-(4'-Chloro benzyl)-2-phenyl-4-(piperidino ethyl) piperazineAusbeute 95 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

31 g. of 1-(4'-chloro benzyl)-2-phenyl piperazine prepared according to Example 2 B), 25 g. of piperidino ethylchloride, 20 g. of triethylamine, and 250 cc. of acetone are boiled under reflux for 18 hours. The filtered reaction solution is freed of its solvent by concentration by evaporation. The residue is dissolved in benzene. The benzene solution is washed with water. After drying and distilling off the solvent, the base is obtained in the form of a viscous, yellow oil on distillation at 210° C./0.06 Torr. The oil crystallizes on trituration with isopropanol. After twice recrystallizing the crystals from n-heptane (41 g. of yellow crystals of the melting point 85°-87° C.) are obtained. The yield is 95 % of the theoretical yield.

Aufarbeitung

  1. temperatureunder reflux for 18 hours
  2. customThe filtered reaction solution
  3. concentrationis freed of its solvent by concentration by evaporation
  4. dissolutionThe residue is dissolved in benzene
  5. washThe benzene solution is washed with water
  6. customAfter drying
  7. distillationdistilling off the solvent
  8. customthe base is obtained in the form of a viscous, yellow oil
  9. distillationon distillation at 210° C./0.06 Torr
  10. customThe oil crystallizes on trituration with isopropanol
  11. customAfter twice recrystallizing the crystals from n-heptane (41 g
  12. customof yellow crystals of the melting point 85°-87° C.) are obtained

Quellen und Nachweise

ORD-Eintrag
ord-279652a72c0f40d0bb3ef2772d6d5ceb
Quelldatensatz
uspto-grants-1976_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US03935214

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