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Triethylamine → 1192720-23-2

HRID 880518
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 880518
[CH3:1][N:2]1[C:6]([CH3:7])=[CH:5][C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:3]1[C:14](=[O:18])[C:15](Cl)=[O:16].[CH3:19][C:20]1[CH:25]=[C:24]([CH3:26])[N:23]=[C:22]([N:27]2[CH2:32][CH2:31][N:30]([C:33]3[CH:38]=[CH:37][C:36]([NH2:39])=[CH:35][CH:34]=3)[CH2:29][CH2:28]2)[CH:21]=1.C(N(CC)CC)C>ClCCl.CC(C)=O>[CH3:1][N:2]1[C:6]([CH3:7])=[CH:5][C:4]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:3]1[C:14](=[O:18])[C:15]([NH:39][C:36]1[CH:35]=[CH:34][C:33]([N:30]2[CH2:31][CH2:32][N:27]([C:22]3[CH:21]=[C:20]([CH3:19])[CH:25]=[C:24]([CH3:26])[N:23]=3)[CH2:28][CH2:29]2)=[CH:38][CH:37]=1)=[O:16]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 8471TriethylamineHCID 668513514-[4-(4,6-Dimethyl-2-pyridyl)piperazin-1-yl]anilineHCID 866546741192719-19-9

Produkt 1

HCID 442088481192720-23-2Ausbeute 75,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittel
HCID 6344
Dichloromethane
Lösungsmittel
2×

Reaktionsbedingungen

Temperatur
47.5 °C

Versuchsvorschrift

A solution of (1,5-dimethyl-3-phenyl-1H-pyrrol-2-yl)-oxo-acetyl chloride (46 g, 0.176 mol) in dry dichloromethane (300 mL) was added to a solution of 4-[4-(4,6-dimethyl-pyridin-2-yl)-piperazin-1-yl]-phenylamine (40 g, 0.140 mol) and triethylamine (14.2 g, 0.140 mol) in dry dichloromethane (300 mL) over 15 min. After stirring for 1 h the reaction mixture was quenched into water (200 mL) and the organic phase separated. The aqueous layer was extracted with dichloromethane (2×50 mL) and the combined organic layers were washed successively with water (2×200 mL), brine (2×100 mL), dried over anhydrous sodium sulfate and concentrated to give a solid. This was dissolved in acetone (580 mL) and silica gel was added (72.5 g, 100-200 mesh). The mixture was stirred at room temperature for 1 h, filtered and the solids washed with acetone (75 mL). The silica treatment was repeated a second time. The filtrate was concentrated to ˜300 mL (˜4 vols), activated carbon (8 g) was added and heated at reflux for 15 min. The mixture was cooled to 45-50° C. and filtered over celite, washing with acetone (75 mL). The solution was again concentrated to ˜300 mL and petroleum ether (725 mL, 10 vols) was added, slowly, at reflux. The resulting suspension was cooled to room temperature, stirred for 15 min, then cooled to 0° C. and stirred for 1 h. The solid was filtered off, washed with petroleum ether (150 mL) and dried under vacuum to afford 2-(1,5-dimethyl-3-phenyl-1H-pyrrol-2-yl)-N-{4-[4-(4,6-dimethyl-pyridin-2-yl)-piperazin-1-yl]-phenyl}-2-oxo-acetamide (53.5 g, 74%) as a yellow solid.

Aufarbeitung

  1. customwas quenched into water (200 mL)
  2. customthe organic phase separated
  3. extractionThe aqueous layer was extracted with dichloromethane (2×50 mL)
  4. washthe combined organic layers were washed successively with water (2×200 mL), brine (2×100 mL)
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customto give a solid
  8. additionsilica gel was added (72.5 g, 100-200 mesh)
  9. stirringThe mixture was stirred at room temperature for 1 h
  10. filtrationfiltered
  11. washthe solids washed with acetone (75 mL)
  12. concentrationThe filtrate was concentrated to ˜300 mL (˜4 vols), activated carbon (8 g)
  13. additionwas added
  14. temperatureheated
  15. temperatureat reflux for 15 min
  16. filtrationfiltered over celite
  17. washwashing with acetone (75 mL)
  18. concentrationThe solution was again concentrated to ˜300 mL and petroleum ether (725 mL, 10 vols)
  19. additionwas added
  20. temperatureslowly, at reflux
  21. temperatureThe resulting suspension was cooled to room temperature
  22. stirringstirred for 15 min
  23. temperaturecooled to 0° C.
  24. stirringstirred for 1 h
  25. filtrationThe solid was filtered off
  26. washwashed with petroleum ether (150 mL)
  27. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-1dcdd63af92c4ecb8bec5ebf7242aade
Quelldatensatz
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08993574B2

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