反应详情

温度

80 °C

A mixture of N-(3,5-Bis-trifluoromethyl-benzyl)-N-(9-bromo-7-trifluoromethyl-2,3,4,5-tetrahydro-1H-benzo[b]azepin-5-yl)-acetamide (0.0830 g, 0.144 mmol), methyl boronic acid (0.0260 g, 0.432 mmol) and cesium fluoride (0.0770 mg, 0.504 mmol) in dioxane (2.00 ml) was purged with nitrogen for 10 minutes. To it was added PdCl2(dppf) (0.0170 g) in one portion. The mixture was heated at 80° C. overnight. The solid was removed by filtration, washed with ethyl acetate (30.0 ml) and the filtrate was concentrated in vacuo. Purification by silica gel chromatography (gradient eluent, 0-40% ethyl acetate in hexane) provided the titled compound (0.0460 g, 63%) as white solid. MS (ES+): 513 (M+H).

1. customwas purged with nitrogen for 10 minutes
2. additionTo it was added PdCl2(dppf) (0.0170 g) in one portion
3. customThe solid was removed by filtration
4. washwashed with ethyl acetate (30.0 ml)
5. concentrationthe filtrate was concentrated in vacuo
6. customPurification by silica gel chromatography (gradient eluent, 0-40% ethyl acetate in hexane)