反应详情

Chill a solution of nitrosonium tetrafluoroborate (0.074 g, 0.63 mmol), hydrogen fluoride-pyridine (0.250 mL) in dichloromethane (2 mL) in aplastic bottle. Add a solution of N-methyl-5-(2-phenyl-[1,3]dithian-2-yl)-N-propyl-isophthalamic acid methyl ester (0.123 g, 0.286 mmol) in dichloromethane (1 mL) to the bottle and stir at room temperature for 2 h. Dilute the solution with dichloromethane (5 mL) and filter though a pad of magnesium sulfate and aluminum oxide. Wash solid with ethyl acetate (50 mL), concentrate and purify (silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes) to give the title compound (42%).

1. filtrationfilter though a pad of magnesium sulfate and aluminum oxide
2. washWash solid with ethyl acetate (50 mL)
3. concentrationconcentrate
4. custompurify
5. wash(silica gel chromatography, eluting with 20:80 to 30:70 ethyl acetate:hexanes)