Reaktion #9863

Reaktionsgleichung

2-Amino-thiophene-3-carboxlic acid amide

potassium ethylxanthate

→

title compound

Ausbeute 69.5%

2-Thioxo-2,3-dihydro-1H-thieno[2,3-d]pyrimidin-4-one

Ausbeute 69.5%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe solvent (DMF) was removed on the rotovap under high vacuum at 90° C
2. 2
   workup.ADDITIONThe residue was diluted with 600 mL of aqueous citric acid (5%)
3. 3
   Temperaturcooled to 0° C.
4. 4
   FiltrationThe tan powder was filtered
5. 5
   Sonstigedried overnight

Vorschrift

2-Amino-thiophene-3-carboxlic acid amide (28.4 g, 0.2 mol) and potassium ethylxanthate (96 g, 3 eq) were mixed together and added to DMF (1000 mL). The resulting mixture was heated to 150° C. for about six hours. The solvent (DMF) was removed on the rotovap under high vacuum at 90° C. The residue was diluted with 600 mL of aqueous citric acid (5%) and cooled to 0° C. and stirred for about 30 minutes. The tan powder was filtered and dried overnight to give 25.6 g of the title compound ((M+H)+=185, M.P.>300° C.).

Quelle