Potassium Carbonate → HCID 13374747, Verbindung

HRID 358222

Reaktionsgleichung

Reaktionsgleichung von HRID 358222
Cl.[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.Br[CH2:16][CH2:17][CH2:18][CH2:19]Cl.C(=O)([O-])[O-].[K+].[K+].[N:27]1[NH:28][C:29](=[O:36])[N:30]2[CH:35]=[CH:34][CH:33]=[CH:32][C:31]=12.[Na]>C(Cl)(Cl)Cl.C1(C)C(C)=CC=CC=1>[Cl:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:14][CH2:13][N:12]([CH2:16][CH2:17][CH2:18][CH2:19][N:28]3[C:29](=[O:36])[N:30]4[CH:35]=[CH:34][CH:33]=[CH:32][C:31]4=[N:27]3)[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1

Komponenten

7

Edukt 4

HCID 11430Potassium CarbonateHCID 256811-(3-Chlorophenyl)piperazine monohydrochlorideHCID 813641-Bromo-4-chlorobutaneHCID 70507128Sodium 1,2,4-Triazolo[4,3-a]pyridin-3(2H)-one

Produkt 1

HCID 13374747HCID 13374747, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6212ChloroformLösungsmittelHCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

A mixture of 8.0 g. (0.0343 mole) of 1-(3-chlorophenyl)piperazine hydrocloride, 5.88 g. (0.0343 mole) of 1-bromo-4-chlorobutane, 9.48 g. (0.9686 mole) of finely powdered potassium carbonate, and 200 ml. of dry xylene was refluxed for 22 hr. To this mixture there was then added 5.39 g. (0.0343 mole) of sodium 1,2,4-triazolo[4,3-a]pyridin-3(2H)-one, and the resulting suspension was refluxed an additional 72 hr. The mixture was then cooled, diluted with 200 ml. of chloroform, stirred for 15 min. and filtered. The clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure. The residue was recrystallized from ET2O--EtOH--CHCl3 to afford 2.31 g. (43%) of the desired product, m.p. 122°-123°.

Aufarbeitung

  1. additionA mixture of 8.0 g
  2. additionTo this mixture there was then added 5.39 g
  3. temperatureThe mixture was then cooled
  4. additiondiluted with 200 ml
  5. filtrationfiltered
  6. concentrationThe clear filtrate was concentrated to an oil (9.8 g.) under reduced pressure
  7. customThe residue was recrystallized from ET2O
  8. customEtOH--CHCl3 to afford 2.31 g

Quellen und Nachweise

ORD-Eintrag
ord-9921cd8d05fa42deba4b5fc11d0e9396
Quelldatensatz
uspto-grants-1984_08
Patentnummer
US04465683

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