Reacción #2262561

Ecuación de reacción

3H-thieno[3,2-d]pyrimidine-4-one

dimethylformamide

dichloroethane

oxalyl chloride

→

title compound

Rendimiento 99.0%

4-chloro-thieno[3,2-d]pyrimidine

Rendimiento 99.0%

Disolventes

water

Condiciones de reacción

Tratamiento posterior

1. 1
   Otroto 0° C.
2. 2
   Otroto form
3. 3
   Otrowas lowed to room temperature
4. 4
   Extracciónthe reaction mixture was extracted
5. 5
   Secadodried with anhydrous magnesium sulfate
6. 6
   ConcentraciónAfter concentrated under vacuum, trituration

Procedimiento

After dimethylformamide (15.4 ml, 197.13 mmol) was added into 150 ml of dichloroethane with lowering the temperature to 0° C., oxalyl chloride (25 4 ml, 295.70 mmol) was slowly added. When white gel type started to form, 3H-thieno[3,2-d]pyrimidine-4-one (15 g, 98.57 mmol) was added. After 2.5 hours of reflex of the reaction mixture, the temperature was lowed to room temperature. After adding water, the reaction mixture was extracted using dichloromethane (3×300 ml) and dried with anhydrous magnesium sulfate. After concentrated under vacuum, trituration was carried out with 200 ml of hexane and the title compound (16.7 g, 99%) was obtained as a dark brown solid.

Fuente