反应详情

A mixture of 1-(2,3-dimethylphenyl)-1-propanone (11.2 g), paraformaldehyde (2.70 g), pyrrolidine-hydrochloride (9.7 g), and hydrochloric acid (0.5 ml) in isopropyl alcohol (15 ml) was refluxed for 8.5 hours. The reaction mixture was evaporated in vacuo to give the residue. The residue was dissolved in water and then washed with ethyl acetate. The aqueous layer was extracted with dichloromethane and then dried over anhydrous magnesium sulfate. The mixture was filtered and then the filtrate was evaporated in vacuo to give the residue. The residue was recrystallized from CH2Cl2 --AcOEt to give 2-methyl-1-(2,3-dimethylphenyl)-3-pyrrolidino-1-propanone hydrochloride (13.1 g, Y: 64.7%) as colorless prisms, m.p. 149°-151° C. ##STR319##

1. temperaturewas refluxed for 8.5 hours
2. customThe reaction mixture was evaporated in vacuo
3. customto give the residue
4. washwashed with ethyl acetate
5. extractionThe aqueous layer was extracted with dichloromethane
6. dry with materialdried over anhydrous magnesium sulfate
7. filtrationThe mixture was filtered
8. customthe filtrate was evaporated in vacuo
9. customto give the residue
10. customThe residue was recrystallized from CH2Cl2