反应详情

A suspension of 1-(4-(4-methoxy-3-methylbenzoyl)piperidin-1-yl)ethanone (5.45 g, 19.8 mmol) in 6 N HCl (40 mL) was heated to reflux for 12 h then concentrated in vacuo to a light purple solid. The material was taken up in ˜100 mL MeOH with heating and sonication, concentrated in vacuo to ˜25 mL, added diethyl ether (˜200 mL) to form white precipitate and a purple aqueous layer. The aqueous layer was removed via a pipet and concentrated in vacuo. The suspension was decanted through filter to recover a white solid (1.30 g). The aqueous material was concentrated in vacuo to form a purplish oil which was taken up in diethyl ether and the resulting suspension was filtered (0.82 g). The filtrate was concentrated in vacuo to a purple oil. The solid material was confirmed to be the title compound. Calculated molecular formula=C14H19NO2=233.31. found MS (ESI) m/e 233.9 (M+H+)

1. temperaturewas heated
2. temperatureto reflux for 12 h
3. concentrationthen concentrated in vacuo to a light purple solid
4. temperaturewith heating
5. customsonication
6. concentrationconcentrated in vacuo to ˜25 mL
7. additionadded diethyl ether (˜200 mL)
8. customto form white precipitate
9. customThe aqueous layer was removed via a pipet
10. concentrationconcentrated in vacuo
11. customThe suspension was decanted
12. filtrationthrough filter
13. customto recover a white solid (1.30 g)
14. concentrationThe aqueous material was concentrated in vacuo
15. customto form a purplish oil which
16. filtrationthe resulting suspension was filtered (0.82 g)
17. concentrationThe filtrate was concentrated in vacuo to a purple oil