Acetic Acid → 7,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dione

HRID 595071Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 595071
C(S[C:4]1[NH:5][C:6](=[O:14])[C:7]2[S:13][CH2:12][CH2:11][CH2:10][C:8]=2[N:9]=1)C.Cl.CC(O)=[O:18]>O>[NH:9]1[C:8]2[CH2:10][CH2:11][CH2:12][S:13][C:7]=2[C:6](=[O:14])[NH:5][C:4]1=[O:18]

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 135535910HCID 135535910, Verbindung

Produkt 1

HCID 99899257,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dioneAusbeute 72 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a suspension of 2-(ethylthio)-7,8-dihydro-3H-thiopyrano[3,2-d]pyrimidin-4(6H)-one (4.5 g, 19.7 mmol) in water (20 mL) was added 3.0 mL of conc. HCl and 6.0 mL of AcOH. The mixture was heated to reflux and stirred overnight. The reaction was cooled and the solid that formed was collected by filtration, washed with water and methanol, evaporated and dried to obtain 7,8-dihydro-1H-thiopyrano[3,2-d]pyrimidine-2,4(3H,6H)-dione as a white solid (2.6 g, 72%). Without further purification, the crude product was used directly in the next step.

Aufarbeitung

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. temperatureThe reaction was cooled
  4. customthe solid that formed
  5. filtrationwas collected by filtration
  6. washwashed with water and methanol
  7. customevaporated
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-ed231be56d2f4202bd2a148f44cad9c0
Quelldatensatz
uspto-grants-2016_01
Patentnummer
US09242993B2

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