Ammonium Hydroxide → HCID 20378679, Verbindung

HRID 437949Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 437949
[CH3:1][N:2]1[CH2:16][CH2:15][N:5]2[C:6]3[C:11]([NH:12][C:13](=O)[CH:4]2[CH2:3]1)=[CH:10][CH:9]=[CH:8][CH:7]=3.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[NH4+].C(O)(=O)/C=C/C(O)=O>CC(C)=O.O1CCCC1>[CH3:1][N:2]1[CH2:16][CH2:15][N:5]2[C:6]3[C:11]([NH:12][CH2:13][CH:4]2[CH2:3]1)=[CH:10][CH:9]=[CH:8][CH:7]=3

Komponenten

7

Edukt 4

HCID 14923Ammonium HydroxideHCID 444972Fumaric Acid2×HCID 20378670HCID 20378670, VerbindungHCID 21226445Aluminium lithium hydride

Produkt 1

HCID 20378679HCID 20378679, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of 7.1 g. of 2,3,4,4a-tetrahydro-3-methyl- 1H-pyrazino[1,2-a]quinoxalin-5(6H)-one, 3.5 g. of lithium aluminum hydride and 450 ml. of dry tetrahydrofuran is refluxed for 20 hours under a nitrogen atmosphere. The mixture is cooled and 20 ml. of concentrated ammonium hydroxide is carefully added. The mixture is filtered and the filter cake is washed with isopropanol. The filtrate is concentrated to give 5.7 g. of product as a viscous oil. A 3.5 g. portion is dissolved in acetone and treated with a saturated solution of fumaric acid in acetone. Filtration gives 3.3 g. of the product as the fumaric acid salt, m.p. 178°-188°. Recrystallization from isopropanol gives 2.1 g. of salt, m.p. 186°-188° .

Aufarbeitung

  1. additionA mixture of 7.1 g
  2. temperatureThe mixture is cooled
  3. filtrationThe mixture is filtered
  4. washthe filter cake is washed with isopropanol
  5. concentrationThe filtrate is concentrated
  6. customto give 5.7 g
  7. filtrationFiltration
  8. customgives 3.3 g
  9. customRecrystallization from isopropanol
  10. customgives 2.1 g

Quellen und Nachweise

ORD-Eintrag
ord-750dd0422c6a4e77a9d8f864237df011
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04032639

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