反应详情

温度

50 °C

A mixture of 4-[4-Bromo-1-(2-hydroxy-ethyl)-1H-imidazol-2-yl]-piperidine-1-carboxylic acid tert-butyl ester (2000.00 mg; 5.34 mmol; 1.00 eq.), 2-(4-fluoro-3-trifluoromethyl-phenyl)-4,4,5,5-tetramethyl-[1,3,2]dioxaborolane (1233.97 mg; 8.02 mmol; 1.50 eq.), mg; 0.53 mmol; 0.10 eq.) and Cs2CO3 (3483 mg, 10.69 mmol) in dioxane 15 ml and water 1.5 ml was purged with argon, added Pd(0)(tBu3)2 (273 mg, 0.53 mmol), stirred at 50° C. for overnight. LC-MS showed desired as major product. Diluted reaction solution with EA 70 ml, washed with brine 30mIX2, separated out organic layer, dried, removed off solvent, got crude product, which was subjected to biotage NASP column (100 g), elated with 40-100% EA in hexane and contained 0.5% TEA in EA, collected title compound 1650 mg, 76%

1. additionDiluted
2. washwashed with brine 30mIX2
3. customseparated out organic layer
4. customdried
5. customremoved off solvent
6. customcollected title compound 1650 mg, 76%