反应详情

To 10.56 g 5,6,7,8-tetrahydro[1]benzothieno[2,3-d]pyrimidin-4(3H)-one (0.51 mol) and 10 mL dimethylaniline was added, in one portion, 50 mL POCl3. The mixture was heated to reflux for 5 h under argon, cooled and the excess POCl3 was removed by concentration in vacuo. The residue was poured into 200 g ice and neutralized with satd Na2CO3. The resulting blue-gray gum was filtered, washed with water and crystallized from ethanol to give 7.03 g (0.031 mol) of product.

1. temperatureThe mixture was heated
2. temperatureto reflux for 5 h under argon
3. temperaturecooled
4. customthe excess POCl3 was removed by concentration in vacuo
5. additionThe residue was poured into 200 g ice and neutralized with satd Na2CO3
6. filtrationThe resulting blue-gray gum was filtered
7. washwashed with water
8. customcrystallized from ethanol