反应详情

A mixture of N-[(4-benzyl-2-morpholinyl)methyl]phthalimide (162 g), 85% hydrazine hydrate (43.3 g), and ethanol (100 ml) is refluxed with stirring for 20 minutes. The reaction mixture is filtered, and the filtrate is diluted with water and extracted with chloroform. The organic layer is separated, washed with a small amount of water and then with saturated aqueous sodium chloride solution, dried over magnesium sulfate, and filtered. To the filtrate is added slowly acetic anhydride (98.3 g), and the resulting mixture is stirred at 25° C. for 2 hours. The reaction mixture is washed successively with aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution, and dried over magnesium sulfate. The solvent is distilled off under reduced pressure, and the residue is recrystallized from toluene to give the title compound (101 g), mp 110°-111° C.

1. temperatureis refluxed
2. filtrationThe reaction mixture is filtered
3. additionthe filtrate is diluted with water
4. extractionextracted with chloroform
5. customThe organic layer is separated
6. washwashed with a small amount of water
7. dry with materialwith saturated aqueous sodium chloride solution, dried over magnesium sulfate
8. filtrationfiltered
9. additionTo the filtrate is added slowly acetic anhydride (98.3 g)
10. stirringthe resulting mixture is stirred at 25° C. for 2 hours
11. washThe reaction mixture is washed successively with aqueous sodium hydroxide solution, water and saturated aqueous sodium chloride solution
12. dry with materialdried over magnesium sulfate
13. distillationThe solvent is distilled off under reduced pressure
14. customthe residue is recrystallized from toluene