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Triethylamine → 4-Piperidinol, 4-(p-chlorophenyl)-1-(3-(10,11-dihydro-5H-dibenz(b,f)azepin-5-yl)propyl)-, hydrochloride, hydrate (2:2:1)

HRID 1166411
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1166411
[CH:1]1[C:11]2[CH2:10][CH2:9][C:8]3[CH:12]=[CH:13][CH:14]=[CH:15][C:7]=3[N:6]([CH2:16][CH2:17][CH2:18]O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.CS([Cl:31])(=O)=O.S([O-])(=O)(=O)C.[Cl:37][C:38]1[CH:43]=[CH:42][C:41]([C:44]2([OH:50])[CH2:49][CH2:48][NH:47][CH2:46][CH2:45]2)=[CH:40][CH:39]=1.C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.C(#N)C.O>[ClH:31].[Cl:37][C:38]1[CH:43]=[CH:42][C:41]([C:44]2([OH:50])[CH2:45][CH2:46][N:47]([CH2:18][CH2:17][CH2:16][N:6]3[C:7]4[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=4[CH2:9][CH2:10][C:11]4[CH:1]=[CH:2][CH:3]=[CH:4][C:5]3=4)[CH2:48][CH2:49]2)=[CH:40][CH:39]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 6

HCID 8471TriethylamineHCID 11430Potassium CarbonateHCID 31297Methanesulfonyl chlorideHCID 382824-(4-Chlorophenyl)-4-hydroxypiperidineHCID 85257MethanesulfonateHCID 110214143-(10,11-dihydro-5H-dibenz[b,f]azepin-5-yl)-1-propanol

Produkt 1

HCID 201560
4-Piperidinol, 4-(p-chlorophenyl)-1-(3-(10,11-dihydro-5H-dibenz(b,f)azepin-5-yl)propyl)-, hydrochloride, hydrate (2:2:1)
Ausbeute 61 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittel2×HCID 1140TolueneLösungsmittelHCID 6342AcetonitrileLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

To a stirred solution of the above alcohol (1.01 g, 0.004 mol) and triethylamine (1.02 g, 0.010 mol) in toluene (25 ml) at 0° C., methanesulfonyl chloride (0.6 ml, 0.0077 mol) was added dropwise over 10 minutes. The resulting mixture, was stirred at 0° C. for 1.5 h. Water (50 ml) was added and the phases were separated. The aqueous phase was extracted with toluene (50 ml), and the combined organic phases were washed with brine (2×50 ml), dried (MgSO4) and concentrated in vacuo. The crude mesylate was mixed with 4-(4-chlorophenyl)piperidin-4-ol (0.81 g, 0.004 mol) and potassium carbonate (1.08 g, 0.008 mol) in acetonitrile (9 ml) and heated at reflux temperature for 6 h. The reaction mixture was left stirring at room temperature for 2 days. Water (50 ml) was added and the mixture was extracted with ethyl acetate (3×15 ml), washed with brine (2×20 ml), dried (MgSO4) and concentrated in vacuo. Water (50 ml) was added and the mixture was acidified by addition of concentrated hydrochloric acid (3 ml). The aqueous solution was extracted with dichloromethane (2×20 ml), washed with brine (2×20 ml), dried (MgSO4) and concentrated in vacuo. The resulting oil was dissolved in a mixture of ethyl acetate (15 ml) and methanol (2 ml). Heptane was added in small portions, just until the solution turned slightly turbid. After 4 h, crystals were filtered off, washed with heptane and dried, affording 1.1 g (61%) of the title compound as a solid.

Aufarbeitung

  1. customthe phases were separated
  2. extractionThe aqueous phase was extracted with toluene (50 ml)
  3. washthe combined organic phases were washed with brine (2×50 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. temperatureheated
  7. temperatureat reflux temperature for 6 h
  8. waitThe reaction mixture was left
  9. stirringstirring at room temperature for 2 days
  10. extractionthe mixture was extracted with ethyl acetate (3×15 ml)
  11. washwashed with brine (2×20 ml)
  12. dry with materialdried (MgSO4)
  13. concentrationconcentrated in vacuo
  14. additionWater (50 ml) was added
  15. additionthe mixture was acidified by addition of concentrated hydrochloric acid (3 ml)
  16. extractionThe aqueous solution was extracted with dichloromethane (2×20 ml)
  17. washwashed with brine (2×20 ml)
  18. dry with materialdried (MgSO4)
  19. concentrationconcentrated in vacuo
  20. dissolutionThe resulting oil was dissolved in a mixture of ethyl acetate (15 ml) and methanol (2 ml)
  21. additionHeptane was added in small portions, just until the solution
  22. waitAfter 4 h
  23. filtrationcrystals were filtered off
  24. washwashed with heptane
  25. customdried

Quellen und Nachweise

ORD-Eintrag
ord-2e257e1c17de459eb731695ae1aef847
Quelldatensatz
uspto-grants-2003_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US06613791B1

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