反应详情

To a suspension of (4-methoxyphenyl)(piperidin-4-yl)methanone (34 g, 155 mmol) and (R)-2-oxopyrrolidin-3-yl methanesulfonate (34.7 g, 194 mmol) in acetonitrile (388 mL) at room temperature was added DIPEA (108 mL, 620 mmol) and the reaction was heated to 60 C for 29 h then allowed to cool to room temperature and stirred for an additional 24 h. The reaction mixture was concentrated in vacuo to afford a waxy solid which was taken up in ethyl acetate (300 mL) and sonicated. The mixture was filtered and the resulting white solid was washed with ethyl acetate (200 mL) to yield 21.05 g. The combined filtrates were concentrated and purified via silica gel chromatography (330 g isco 0.01% NH4OH 5-10% MeOH/ethyl acetate). Pure fractions were combined, concentrated in vacuo and then taken up in ethyl acetate (80-100 mL) and stirred. A white precipitate formed that was collected by filtration. The filtrate was concentrated to a gold oil, taken up in ethyl acetate to afford a white precipitate that was collected by filtration. A total of 27.7 g of the title material was obtained as a white solid. Calculated MS=302.4. found MS (ESI) m/e 303.4 (M+H+)

1. temperaturethe reaction was heated to 60 C for 29 h
2. concentrationThe reaction mixture was concentrated in vacuo
3. customto afford a waxy solid which
4. customsonicated
5. filtrationThe mixture was filtered
6. washthe resulting white solid was washed with ethyl acetate (200 mL)
7. customto yield 21.05 g
8. concentrationThe combined filtrates were concentrated
9. custompurified via silica gel chromatography (330 g isco 0.01% NH4OH 5-10% MeOH/ethyl acetate)
10. concentrationconcentrated in vacuo
11. stirringstirred
12. customA white precipitate formed
13. filtrationthat was collected by filtration
14. concentrationThe filtrate was concentrated to a gold oil
15. customto afford a white precipitate that
16. filtrationwas collected by filtration