反应详情

Stir a mixture of (3-bromothiophen-2-yl)-(3-methoxyphenyl)methanone (7 g, 0.024 mol), hydroxylamine hydrochloride (3.09 g, 0.048 mol) and pyridine (40 mL) overnight at room temperature, and then heat the mixture (100° C.–105° C.) for four hours. TLC (DCM) shows that the reaction is complete. Quench the reaction mixture with water and extract with ether (three times). Wash the ether phase with HCl (3N) and water, dry (MgSO4), filter and concentrate to yield an oil that solidifies. Recrystallize the solid from ether:hexane to obtain the title compound (6.4 g, 87% Yield), m.p. 102–103° C.

1. temperatureheat the mixture (100° C.–105° C.) for four hours
2. customQuench the reaction mixture with water
3. extractionextract with ether (three times)
4. washWash the ether phase with HCl (3N) and water
5. dry with materialdry (MgSO4)
6. filtrationfilter
7. concentrationconcentrate
8. customto yield an oil
9. customRecrystallize the solid from ether