Reaktion #655321

ord-238baf31883a417f8d6abdd5f1ecee74

Reaktionsgleichung

CCCCn1c(=O)c2[nH]c(Br)nc2n(CCCC)c1=O
1,3-Di-n-butyl-8-bromo xanthine
C1CCNCC1
piperidine
CCCCn1c(=O)c2[nH]c(N3CCCCC3)nc2n(CCCC)c1=O
title product
CCCCn1c(=O)c2[nH]c(N3CCCCC3)nc2n(CCCC)c1=O
1,3-Di-n-butyl-8-piperidino xanthine

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas refluxed for 9 hours
  2. 2
    ExtraktionThe reaction mixture was then extracted with water (4'30 ml), the organic layer
  3. 3
    Trocknendried over anhydrous sodium sulphate
  4. 4
    Sonstigethe solvent removed in vacuo
  5. 5
    SonstigeThe residue was recrystallised from ethanol

Vorschrift

1,3-Di-n-butyl-8-bromo xanthine (2 g, 0.0029 mol) was dissolved in toluene (50 ml). After addition of piperidine (5 g, 0.0058 mol) the mixture was refluxed for 9 hours. The reaction mixture was then extracted with water (4'30 ml), the organic layer dried over anhydrous sodium sulphate and the solvent removed in vacuo. The residue was recrystallised from ethanol to give the title product, yield 0.4 g (20%), m.pt. 221° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06180791B2uspto-grants-2001_01