反应详情

温度

100 °C

rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (213 mg, 0.34 mmol) and palladium acetate (58 mg, 0.26 mmol) were suspended in toluene (10 ml), and after 2-amino-4-picoline (203 mg, 1.88 mmol) and 2-{1-[5-(6-bromopyridin-2-yl)thiazol-2-yl]piperidin-4-yl}-2-methylpropionic acid ethyl ester (748 mg, 1.71 mmol) obtained in Step 2 were sequentially added, cesium carbonate (1.11 g, 3.41 mmol) was added, and the mixture was stirred overnight at 100° C. Water was added to the reaction solution and extracted with ethyl acetate and washed with a saturated brine. The organic layer was dried over anhydrous sodium sulfate and the residue obtained by vacuum concentration was purified by chromatography on silica gel (n-hexane:ethyl acetate=1:1 to 1:3) and the title compound (697 mg, 88%) was obtained.

1. extractionextracted with ethyl acetate
2. washwashed with a saturated brine
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. customthe residue obtained by vacuum concentration
5. customwas purified by chromatography on silica gel (n-hexane:ethyl acetate=1:1 to 1:3)