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Hydrochloric Acid → HCID 20339412, Verbindung

HRID 1395449
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1395449
[F:1][C:2]([F:19])([F:18])[C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]1[CH2:13][CH2:14][NH:15][CH2:16][CH:8]1[C:7](=[O:17])[NH:6]2.[CH:20]([C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)=[CH2:21].CO.Cl>C(O)C.C(O)(=O)C>[N:23]1[CH:24]=[CH:25][CH:26]=[CH:27][C:22]=1[CH2:20][CH2:21][N:15]1[CH2:14][CH2:13][N:9]2[C:10]3[C:5]([NH:6][C:7](=[O:17])[CH:8]2[CH2:16]1)=[CH:4][C:3]([C:2]([F:18])([F:1])[F:19])=[CH:12][CH:11]=3
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 75212-VinylpyridineHCID 203394142,3,4,4a-Tetrahydro-8-(trifluoromethyl)-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one

Produkt 1

HCID 20339412HCID 20339412, VerbindungAusbeute 71 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 176
Acetic Acid
Lösungsmittel
HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 8.5 g. (0.03 mole) of 2,3,4,4a-tetrahydro-8-trifluoromethyl-1H-pyrazino[1,2-a]quinoxalin-5(6H)-one and 17.5 g. (0.16 mole) of 2-vinylpyridine in 250 ml. of methanol containing 7 ml. acetic acid was heated under reflux for 20 hours. The reaction mixture was cooled, and the solvent was removed under reduced pressure. The residue was precipitated with 1 l. of water. The product was filtered and recrystallized from methanol-water to yield 10.1 g. of free base. 4.5 G. of this free base was dissolved in 150 ml. of absolute ethanol and treated with dry hydrogen chloride saturated ether solution. The product hydrochloride was filtered and recrystallized two times from methanol-ether to give 4 g. (71%) of the title compound as the dihydrochloride salt, m.p. 194°-196° C.

Aufarbeitung

  1. temperatureunder reflux for 20 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent was removed under reduced pressure
  4. customThe residue was precipitated with 1 l
  5. filtrationThe product was filtered
  6. customrecrystallized from methanol-water
  7. customto yield 10.1 g
  8. dissolutionof this free base was dissolved in 150 ml
  9. filtrationThe product hydrochloride was filtered
  10. customrecrystallized two times from methanol-ether
  11. customto give 4 g

Quellen und Nachweise

ORD-Eintrag
ord-957a35fd298a4cc28c3e29bf5720b8a3
Quelldatensatz
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04203987

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