反应详情

A mixture of Z-(1H-Pyrrol-2-ylmethylene)-1,3-dihydro-indol-2-one (120 mg, 0.57 mmol), paraformaldehyde (32 mg, 1.1 mmol), and morpholine (62.2 μL, 0.71 mmol) in 8.0 mL of 20% dioxane in EtOH was heated at reflux for 19.5 h. The reaction mixture was concentrated and paraformaldehyde (10.0 mg, 0.33 mmol), morpholine (15 μL, 0.17 mmol) and EtOH (7 mL) was added. The reaction mixture refluxed for 24 h. The reaction mixture was cooled to room temperature and concentrated. The residue was dissolved in 15 mL of CHCl3 and treated with activated charcoal. The resulting suspension was filtered and the filtrate concentrated. The residue was crystallization from ethyl acetate/hexane to give the title compound (88.0 mg, 50%) as a bright yellow solid.

1. temperaturewas heated
2. temperatureat reflux for 19.5 h
3. concentrationThe reaction mixture was concentrated
4. temperatureThe reaction mixture refluxed for 24 h
5. concentrationconcentrated
6. dissolutionThe residue was dissolved in 15 mL of CHCl3
7. additiontreated with activated charcoal
8. filtrationThe resulting suspension was filtered
9. concentrationthe filtrate concentrated
10. customcrystallization from ethyl acetate/hexane