Methane → HCID 178477337, Verbindung

HRID 2287751Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2287751
O=[C:2]1[C:11]2[C:6](=[N:7][C:8]([S:12][CH2:13][CH3:14])=[N:9][CH:10]=2)[N:5]=[CH:4][NH:3]1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:16].N1C=CC=CC=1.C>[OH-].[Na+]>[S:16]=[C:2]1[C:11]2[C:6](=[N:7][C:8]([S:12][CH2:13][CH3:14])=[N:9][CH:10]=2)[N:5]=[CH:4][NH:3]1

Komponenten

6

Edukt 4

HCID 297MethaneHCID 1049Pyridine2×HCID 14817Phosphorus sulfide (P2S5)HCID 135424359NSC403089

Produkt 1

HCID 178477337HCID 178477337, VerbindungAusbeute 95,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

A mixture of 4-oxo-7-ethylthio-3H-pyrimido[4,5-d]pyrimidine (1.33 g, 6.7 mmol), P2S5 (1.48 g, 6.6 mmol) and pyridine (15 mL) is refluxed under N2 for 3 h. The pyridine is then stripped under reduced pressure, and the residue is dissolved in NaOH solution (0.5M, 75 mL) and boiled with charcoal. After filtration, the filtrate is neutralized with acetic acid to generate a gold brown solid. Buchner filtration and drying in a vacuum oven affords 4-thiono-7-ethylthio-3H-pyrimido[4,5-d]pyrimidine (1.42 g, 95%). 1H NMR (DMSO) δ 9.47 (1H, s), 8.46 (1H, s), 3.20 (2H, q, J=7.3 Hz), 1.35 (3H, t, J=7.3 Hz).

Aufarbeitung

  1. temperatureis refluxed under N2 for 3 h
  2. filtrationAfter filtration
  3. filtrationBuchner filtration
  4. customdrying in a vacuum oven

Quellen und Nachweise

ORD-Eintrag
ord-eb7e8e8741ed42509c9bfd9bf8453198
Quelldatensatz
uspto-grants-2000_07
Patentnummer
US06084095

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