Sulfuric Acid → HCID 53936879, Verbindung

HRID 845494Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 845494
[CH2:1]([CH:5]1[CH2:13][CH2:12][CH:11]2[CH:7]([C:8](=O)[C:9](=[O:14])[NH:10]2)[CH2:6]1)[CH2:2][CH2:3][CH3:4].[H][H].S(=O)(=O)(O)O.C([O-])(=O)C.[Na+]>C(O)(=O)C.[Pd].[Rh]>[CH2:1]([CH:5]1[CH2:13][CH2:12][CH:11]2[CH:7]([CH2:8][C:9](=[O:14])[NH:10]2)[CH2:6]1)[CH2:2][CH2:3][CH3:4]

Komponenten

8

Edukt 4

HCID 1118Sulfuric AcidHCID 517045Sodium AcetateHCID 56994825HCID 56994825, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 53936879HCID 53936879, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 23938PalladiumKatalysator2×HCID 23948RhodiumKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

For example, a solution of 5-n-butyl-octahydro-2,3-dioxo-1H-indole (III) (43.6 g, 0.214 mole) in acetic acid (250 ml) is treated with hydrogen gas in the presence of 20% Pd/C (2 g). Another 1 g of 20% Pd/C is added and concentrated sulfuric acid (1 ml) is added and the hydrogenation is continued. Ten percent Rh/C (2 g) is added and hydrogenation is continued. The suspension is filtered and sodium acetate (4.9 g, 0.06 mole) is added and the mixture is concentrated at reduced pressure The residue is recrystallized from cyclohexane with the use of activated carbon to yield pure 5-n-butyloctahydro-2-oxo-1H-indole (V) with a mp 109°-111° C.

Aufarbeitung

  1. filtrationThe suspension is filtered
  2. concentrationthe mixture is concentrated at reduced pressure The residue
  3. customis recrystallized from cyclohexane with the use of activated carbon

Quellen und Nachweise

ORD-Eintrag
ord-f17a93c4863749e7a6f3b00ddea050a1
Quelldatensatz
uspto-grants-1988_07
Patentnummer
US04758585

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