Hydrochloric Acid → HCID 18366597, Verbindung

HRID 379574

Reaktionsgleichung

Reaktionsgleichung von HRID 379574
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[CH:9]=[CH:10][S:11][C:5]=2[N:4]([CH2:12][CH:13]([CH3:15])[CH3:14])[C:3]1=[O:16].CN(C)[CH:19]=[O:20].O.Cl>P(Cl)(Cl)(Cl)=O>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2[CH:9]=[C:10]([CH:19]=[O:20])[S:11][C:5]=2[N:4]([CH2:12][CH:13]([CH3:14])[CH3:15])[C:3]1=[O:16]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 6228DimethylformamideHCID 52825273-Methyl-1-(2-methylpropyl)thieno[2,3-d]pyrimidine-2,4(1H,3H)-dione

Produkt 1

HCID 18366597HCID 18366597, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24813Phosphorus oxychlorideLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

1,2,3,4-tetrahydro-3-methyl-1-(2-methylpropyl)-2,4-dioxothieno[2,3-d]pyrimidine (300 mg; WO98/54190) was dissolved in phosphorus oxychloride (4 ml) and dimethylformamide (2 ml) was added. The mixture was then heated to 100° C. with stirring under nitrogen for 1 hour. The mixture was allowed to cool to ambient temperature and then added dropwise to vigorously stirred hot water (˜50° C.), containing a small amount of 2M hydrochloric acid. The mixture formed was allowed to cool to ambient temperature and filtered to give the title compound as a brown solid (210 mg).

Aufarbeitung

  1. temperatureto cool to ambient temperature
  2. customThe mixture formed
  3. temperatureto cool to ambient temperature
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-c19153abb58b4a03ad8847709de0415c
Quelldatensatz
uspto-grants-2001_10
Patentnummer
US06300334B1

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