反応 #1494078
関連文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09168248B2
反応条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
実験手順: To a solution of 2-fluoro-6-(trifluoromethyl)benzamide (500 mg, 2.41 mmol) in diglyme (8.05 mL) was added potassium trimethylsilanolate (1.08 g, 8.45 mmol). The reaction mixture was stirred at 120° C. overnight. The reaction mixture was acidified with 1N HCl (30 mL) and extracted with EtOAc (3×10 mL). The combined organic layers were washed with 10% solution of LiCl in water, dried with MgSO4, filtered and evaporated under reduced pressure. The resulting residue was purified by Combiflash™ chromatography (SiO2, 12 g, elution with 20-40% EtOAc/hexanes over 40 min) to afford the title compound as solid. extracted with EtOAc (3×10 mL) The combined organic layers were washed with 10% solution of LiCl in water dried with MgSO4 filtered evaporated under reduced pressure The resulting residue was purified by Combiflash™ chromatography (SiO2, 12 g, elution with 20-40% EtOAc/hexanes over 40 min)
ソース ID: ord-cd51e396cece4a768396daa6ed2dd6fa