反应详情

A suspension of tert-butyl 2-thioxo-7,8-di-p-tolyl-3a,4-dihydro-[1,3]dioxolo[41,51:4,5] pyrido[2,3-b]pyrazine-5(9bH)-carboxylate (step 3)(14 g, 28.6 mmol) in toluene (400 ml) was treated with tributyltin hydride (16.65 g, 57.2 mmol) and heated at reflux for 2 h. A further portion of tributyltin hydride (10 g) was added and refluxing continued for 6 h. The reaction mixture was left stirring over night at room temperature. The reaction mixture was evaporated to dryness and the iso-hexane (250 ml) was added to the residue. The suspension was stirred for 30 minutes at room temperature and then filtered. The solid was washed with iso-hexane (3×50 ml) to afford the titled compound;

1. temperatureheated
2. temperatureat reflux for 2 h
3. temperaturerefluxing
4. waitThe reaction mixture was left
5. customThe reaction mixture was evaporated to dryness
6. additionthe iso-hexane (250 ml) was added to the residue
7. stirringThe suspension was stirred for 30 minutes at room temperature
8. filtrationfiltered
9. washThe solid was washed with iso-hexane (3×50 ml)