Ammonium formate → FK 1052

HRID 486208Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 486208
O[CH:2]([C:18]1[N:19]=[CH:20][N:21](C(C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[C:22]=1[CH3:23])[CH:3]1[C:16](=[O:17])[N:7]2[C:8]3[C:13]([C:14]([CH3:15])=[C:6]2[CH2:5][CH2:4]1)=[CH:12][CH:11]=[CH:10][CH:9]=3.C([O-])=O.[NH4+]>C(O)(=O)C.[Pd]>[CH3:15][C:14]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]2[C:16](=[O:17])[CH:3]([CH2:2][C:18]3[N:19]=[CH:20][NH:21][C:22]=3[CH3:23])[CH2:4][CH2:5][C:6]=12

Komponenten

5

Edukt 2

HCID 2723923Ammonium formateHCID 150519238,9-dihydro-7-[(hydroxy)(5-methyl-1-trityl-1H-imidazol-4-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one

Produkt 1

HCID 125368FK 1052Ausbeute 76,4 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

To a solution of 8,9-dihydro-7-[(hydroxy)(5-methyl-1-trityl-1H-imidazol-4-yl)methyl]-10-methylpyrido[1,2-a]indol-6(7H)-one (4.6 g) in acetic acid (92 ml) were added 10% palladium on carbon (2.3 g) and ammonium formate (7.89 g), and the mixture was refluxed gently for 3 hours. After being cooled, the catalyst was filtered off. The filtrate was evaporated, and diluted with water (50 ml) and diisopropyl ether (50 ml). Aqueous sodium hydroxide was added to neutralized the solution. Resulted precipitates were collected, and washed with water and diisopropyl ether successively, to give 8,9-dihydro-10-methyl-7-[(5-methyl-1H-imidazol-4-yl)methyl]pyrido[1,2-a]indol-6(7H)-one (1.87 g).

Aufarbeitung

  1. temperaturethe mixture was refluxed gently for 3 hours
  2. temperatureAfter being cooled
  3. filtrationthe catalyst was filtered off
  4. customThe filtrate was evaporated
  5. additiondiluted with water (50 ml) and diisopropyl ether (50 ml)
  6. additionAqueous sodium hydroxide was added
  7. customResulted
  8. customprecipitates
  9. customwere collected
  10. washwashed with water and diisopropyl ether successively

Quellen und Nachweise

ORD-Eintrag
ord-de13585eda784f92b86c3f4209025953
Quelldatensatz
uspto-grants-1994_03
Patentnummer
US05290785

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