反应 #3408002
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08722695B2
反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 4-hydroxy-2-(1-methylethyl)benzonitrile (30 mg) was dissolved in 1 mL of dimethylformamide. 3-(6-fluoro-3-pyridinyl)-5,5-dimethyl-2,4-imidazolidinedione (Intermediate 106, 41.5 mg) and potassium carbonate (51.4 mg, 0.372 mmol) were added. The reaction mixture was stirred at 120° C. during 40 hours. Some diethylether (4 mL) and water (4 mL) were added. The aqueous layer was extracted 4 times with diethylether. The gathered organic layers were dried over sodium sulphate and evaporated giving a residue which was purified by mass directed purification (METHOD H). After evaporation of the fraction, addition of a solution of saturated NaHCO3 (3 mL) and extraction with dichloromethane (four times 4 mL), evaporation afforded the title compound (13 mg). The aqueous layer was extracted 4 times with diethylether The gathered organic layers were dried over sodium sulphate evaporated giving a residue which was purified by mass purification (METHOD H) After evaporation of the fraction, addition of a solution of saturated NaHCO3 (3 mL) and extraction with dichloromethane (four times 4 mL), evaporation
来源 ID: ord-e79eeb3fbcb245bba71f7016187cebbd