反应详情

温度

-100 °C

Under argon, an n-butyllithium solution in hexane (1.55N, 4.6 ml) is added dropwise to a 3,5-dibromo-4-methylpyridine solution (intermediate 10.1, 1.76 g, 7 mmol) kept at −100° C. After stirring for 5 min, DMF (0.84 ml, 1.54 equiv.) is added dropwise. The stirring is maintained for 20 min at −100° C. and then for 1 h at −78° C. An aqueous NH4Cl solution is added and the reaction mixture is extracted with a diethyl ether/water mixture. The yellow solid obtained is purified on silica gel (100 g), eluting with AcOEt/petroleum ether (1/4).

1. customkept at −100° C
2. waitfor 1 h at −78° C
3. extractionthe reaction mixture is extracted with a diethyl ether/water mixture
4. customThe yellow solid obtained
5. customis purified on silica gel (100 g)
6. washeluting with AcOEt/petroleum ether (1/4)