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Hydrochloric Acid → HCID 20339406, Verbindung

HRID 1395453
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1395453
Cl.[CH2:2]1[N:7]2[C:8]3[C:13]([NH:14][C:15](=[O:16])[CH:6]2[CH2:5][NH:4][CH2:3]1)=[CH:12][CH:11]=[CH:10][CH:9]=3.[N:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26]Cl)=[CH:19][CH:18]=1.C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Cl>C(O)C.CC(C)=O.C(N(CC)CC)C>[N:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][CH2:25][CH2:26][N:4]2[CH2:3][CH2:2][N:7]3[C:8]4[C:13]([NH:14][C:15](=[O:16])[CH:6]3[CH2:5]2)=[CH:12][CH:11]=[CH:10][CH:9]=4)=[CH:19][CH:18]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 109539414-(4-Chlorobutyl)pyridineHCID 18377410HCID 18377410, Verbindung

Produkt 1

HCID 20339406HCID 20339406, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 180AcetoneLösungsmittelHCID 702EthanolLösungsmittelHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A solution of 6.2 g. (0.03 mole) of 2,3,4,4a-tetrahydro-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, hydrochloride, 7 g. (0.04 mole) of 4-(4-pyridyl)-1-chlorobutane, 10 g. of potassium carbonate, 5 g. of potassium iodide and 0.5 ml. of triethylamine was stirred and refluxed in 200 ml. of acetone for 48 hours, cooled and filtered. The solvent was removed and the residue was dissolved in methylene chloride. This solution was washed with water and brine, dried over magnesium sulfate and filtered. The solvent was removed and the residue was chromatographed on 500 g. of Silicar, CC-7. Fractions eluted with 10% methanol in ethyl acetate afforded 3.2 g. of free base. 3 G. of the above free base was dissolved in ethanol and treated with dry hydrogen chloride saturated ether. The product hydrochloride was filtered and recrystallized from methanol to give 3.2 g. of the title compound as the dihydrochloride salt, m.p. 281°-283° C.

Aufarbeitung

  1. temperaturerefluxed in 200 ml
  2. temperaturecooled
  3. filtrationfiltered
  4. customThe solvent was removed
  5. dissolutionthe residue was dissolved in methylene chloride
  6. washThis solution was washed with water and brine
  7. dry with materialdried over magnesium sulfate
  8. filtrationfiltered
  9. customThe solvent was removed
  10. customthe residue was chromatographed on 500 g
  11. washFractions eluted with 10% methanol in ethyl acetate
  12. customafforded 3.2 g
  13. filtrationThe product hydrochloride was filtered
  14. customrecrystallized from methanol
  15. customto give 3.2 g

Quellen und Nachweise

ORD-Eintrag
ord-9519b5cb1e74496091edb226acc00108
Quelldatensatz
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04203987

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