Potassium Carbonate → Diethyl [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

HRID 2019

Reaktionsgleichung

Reaktionsgleichung von HRID 2019
[CH2:1]([O:3][CH2:4][N:5]1[C:13]2[C:12](=[O:14])[NH:11][C:10](=[O:15])[N:9]([CH3:16])[C:8]=2[N:7]=[CH:6]1)[CH3:2].Cl[CH2:18][CH2:19][CH2:20][CH2:21][P:22]([O:27][CH2:28][CH3:29])(=[O:26])[O:23][CH2:24][CH3:25].C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH2:1]([O:3][CH2:4][N:5]1[C:13]2[C:12](=[O:14])[N:11]([CH2:18][CH2:19][CH2:20][CH2:21][P:22](=[O:26])([O:27][CH2:28][CH3:29])[O:23][CH2:24][CH3:25])[C:10](=[O:15])[N:9]([CH3:16])[C:8]=2[N:7]=[CH:6]1)[CH3:2]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 137476847-Ethoxymethyl-3-methylxanthineHCID 19689195Diethyl(4-chlorobutyl)phosphonate

Produkt 1

HCID 22446270Diethyl [4-(7-ethoxymethyl-3-methylxanthin-1-yl)butyl]phosphonate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

44.8 g (0.2 mol) of 7-ethoxymethyl-3-methylxanthine were suspended in 500 ml of DMF, treated with 55 g (0.24 mol) of diethyl 4-chlorobutane-phosphonate and 50 g (0.32 mol) of activated potassium carbonate and heated at 70° C. for 4 hours and filtered, the filtrate was concentrated under reduced pressure and the oily residue which remained was taken up in ethyl acetate. filtered again and crystallized from diisopropyl ether.

Aufarbeitung

  1. filtrationfiltered
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. filtrationfiltered again
  4. customcrystallized from diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-84fabc66583e43db913aa7d98ea5cb07
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05728686

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