反应详情

温度

80 °C

A suspension of 2,6-dibromopyridine (12.5 g), 2-amino-4-picoline (32.8 g, 139 mmol), palladium acetate (2.59 g, 11.6 mmol), rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (8.64 g, 13.9 mmol), sodium tert-butoxide (13.3 g, 139 mmol) in toluene (200 ml) was heated and stirred in an Ar stream at 80° C. for 12 hours. Water was added to the reaction solution and the solution was extracted with ethyl acetate. After the organic layer was washed with a saturated brine and dried over anhydrous magnesium sulfate, the residue obtained by vacuum concentration was purified by flash chromatography on silica gel (n-hexane:ethyl acetate=3:1) and subsequently washed with isopropyl ether and the title compound (15.4 g, 51%) was obtained.

1. temperaturewas heated
2. extractionthe solution was extracted with ethyl acetate
3. washAfter the organic layer was washed with a saturated brine
4. dry with materialdried over anhydrous magnesium sulfate
5. customthe residue obtained by vacuum concentration
6. customwas purified by flash chromatography on silica gel (n-hexane:ethyl acetate=3:1)
7. washsubsequently washed with isopropyl ether