3-butyl-1-ethyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione → 3-Butyl-1-ethyl-3,7-dihydro-1H-purine-2,6-dione

HRID 2386649

Reaktionsgleichung

Reaktionsgleichung von HRID 2386649
[CH2:1]([N:5]1[C:13]2[N:12]=[CH:11][N:10](CC3C=CC=CC=3)[C:9]=2[C:8](=[O:21])[N:7]([CH2:22][CH3:23])[C:6]1=[O:24])[CH2:2][CH2:3][CH3:4]>C(O)(=O)C.[OH-].[OH-].[Pd+2]>[CH2:1]([N:5]1[C:13]2[N:12]=[CH:11][NH:10][C:9]=2[C:8](=[O:21])[N:7]([CH2:22][CH3:23])[C:6]1=[O:24])[CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 1

HCID 592995543-butyl-1-ethyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione

Produkt 1

HCID 190037453-Butyl-1-ethyl-3,7-dihydro-1H-purine-2,6-dioneAusbeute 89 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9942167Palladium hydroxideKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

3-butyl-1-ethyl-7-(phenylmethyl)-3,7-dihydro-1H-purine-2,6-dione (0.353 g, 1.08 mmol) was dissolved in acetic acid (30 mL), 20% palladium hydroxide on carbon (0.238 g) was added, and the mixture was shaken under hydrogen (at 50 psi) overnight. The catalyst was removed by filtration through Celite® and washed with acetic acid. The filtrate was concentrated under reduced pressure to yield the title compound (0.227 g, 89%); 1H NMR (400 MHz; CDCl3) δ: 0.97 (3H, t), 1.28 (3H, t), 1.38-1.47 (2H, m), 1.74-1.82 (2H, m), 4.12-4.17 (4H, m), 7.80 (1H, s); m/z 237 [MH+].

Aufarbeitung

  1. customThe catalyst was removed by filtration through Celite®
  2. washwashed with acetic acid
  3. concentrationThe filtrate was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-0a067a23787c4a91b7fde3c971bef117
Quelldatensatz
uspto-grants-2012_09
Patentnummer
US08268839B2

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