反应详情

In a mixture of 50 ml EtOH and 20 ml DMF was dissolved 3.1 g (0.01 mole) of N-(2,6-dichloro-3-pyridylmethyl)phthalimide under heating, followed by addition of 0.75 g (0.015 mole) of H2NNH2.H2O under reflux. After 1 hour of refluxing, EtOH and DMF were distilled off. To the residue were added 10 ml of concentrated hydrochloric acid and 5 ml of water, and the mixture was refluxed for 30 minutes. The resulting crystals were filtered off and the filtrate was neutralized with NaHCO3 and extracted with CH2Cl2 (30 ml×3). The extract was dried over MgSO4 and the solvent was distilled off to give 1.45 g of the title compound as a yellow oil.

1. temperatureunder heating
2. temperatureunder reflux
3. temperatureAfter 1 hour of refluxing
4. distillationEtOH and DMF were distilled off
5. additionTo the residue were added 10 ml of concentrated hydrochloric acid and 5 ml of water
6. temperaturethe mixture was refluxed for 30 minutes
7. filtrationThe resulting crystals were filtered off
8. extractionextracted with CH2Cl2 (30 ml×3)
9. dry with materialThe extract was dried over MgSO4
10. distillationthe solvent was distilled off