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Hydrochloric Acid → 6-Pentyl-6,9-dihydro-5H-[1,2,4]triazolo[3,4-i]purin-5-one

HRID 249767
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 249767
C([N:8]1[C:16]2[C:15]3=[N:17][N:18]=[CH:19][N:14]3[C:13](=[O:20])[N:12]([CH2:21][CH2:22][CH2:23][CH2:24][CH3:25])[C:11]=2[N:10]=[CH:9]1)C1C=CC=CC=1.Cl>C(O)(=O)C.[OH-].[Pd+2].[OH-]>[CH2:21]([N:12]1[C:11]2[N:10]=[CH:9][NH:8][C:16]=2[C:15]2=[N:17][N:18]=[CH:19][N:14]2[C:13]1=[O:20])[CH2:22][CH2:23][CH2:24][CH3:25]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 598538329-Benzyl-6-pentyl-6,9-dihydro-5H-[1,2,4]triazolo[3,4-i]purin-5-one

Produkt 1

HCID 1359846986-Pentyl-6,9-dihydro-5H-[1,2,4]triazolo[3,4-i]purin-5-oneAusbeute 65,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 9942167Palladium hydroxideKatalysator2×HCID 176Acetic Acid
Lösungsmittel

Versuchsvorschrift

To a mixture of 9-benzyl-6-pentyl-6,9-dihydro-5H-[1,2,4]triazolo[3,4-i]purin-5-one (0.25 g, 0.74 mmol) in acetic acid (20 mL) was added palladium hydroxide (0.20 g, 1.4 mmol) under N2. The mixture was shaken under H2 at 60 psi overnight. Since the reaction was not complete, more palladium hydroxide (0.2 g, 1.4 mmol) and concentrated HCl (1 mL) were added. The resulting mixture was shaken under H2 at 60 psi overnight. The reaction solution was filtered and the filtrate was concentrated under vacuum to provide the product as a white solid (0.12 g, 65.6%). LCMS calculated for C11H15N6O (M+H): 247.1. found: 247.1.

Aufarbeitung

  1. stirringThe resulting mixture was shaken under H2 at 60 psi overnight
  2. filtrationThe reaction solution was filtered
  3. concentrationthe filtrate was concentrated under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-acf1ff084c4645c08134ddbe188cad12
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07863285B2

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