tert-Butyl piperazine-1-carboxylate → 4-(7-Benzyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl ester

HRID 1792017Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1792017
[CH2:1]([N:8]1[C:16]2[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH3:19])[C:11]=2[N:10]=[C:9]1Cl)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:23])[CH3:22]>C(OCC)(=O)C>[C:21]([O:25][C:26]([N:28]1[CH2:33][CH2:32][N:31]([C:9]2[N:8]([CH2:1][C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C:16]3[C:15](=[O:17])[NH:14][C:13](=[O:18])[N:12]([CH3:19])[C:11]=3[N:10]=2)[CH2:30][CH2:29]1)=[O:27])([CH3:24])([CH3:22])[CH3:23]

Komponenten

4

Edukt 2

HCID 143452tert-Butyl piperazine-1-carboxylateHCID 9115837-benzyl-8-chloro-3-methyl-1H-purine-2,6(3H,7H)-dione

Produkt 1

HCID 235369514-(7-Benzyl-3-methyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-8-yl)piperazine-1-carboxylic acid tert-butyl esterAusbeute 96,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

7-Benzyl-8-chloro-3-methyl-3,7-dihydropurine-2,6-dione (130 mg) and 1-piperazine carboxylic acid tert-butyl ester (250 mg) were stirred at 150° C. for 1 hour. The reaction mixture was diluted with ethyl acetate, and the resulting suspension was filtered to give white solid. This solid was purified by silica gel column chromatography to obtain 190 mg of the title compound from a fraction eluted with ethyl acetate.

Aufarbeitung

  1. filtrationthe resulting suspension was filtered
  2. customto give white solid
  3. customThis solid was purified by silica gel column chromatography

Quellen und Nachweise

ORD-Eintrag
ord-bae984a2d7ad483fb5f6c32628af5994
Quelldatensatz
uspto-grants-2006_07
Patentnummer
US07074798B2

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