反应 #2947048
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09334267B2
反应条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Add 1-methylpyrrolidine (1.214 mL, 11.54 mmol) in a mixture of prop-1-en-2-yl (2-fluoro-4-methyl-5-(7-methyl-2-(methylthio)pyrido[2,3-d]pyrimidin-6-yl)phenyl)carbamate (0.92 g, 2.31 mmol) and 4,4,4-trifluoro-3,3-dimethylbutan-1-amine hydrochloride (0.487 g, 2.54 mmol) in THF (23 mL) and heat at 65° C. for 4 h. Cool the mixture to RT, dilute with EtOAc, wash with brine (2×), dry over MgSO4, concentrate to dryness and purify via silica gel chromatography (0-50% EtOAc/Hexanes) to afford the title compound (860 mg, 75% yield). MS (m/z): 496.2 (M+1). Cool the mixture to RT wash with brine (2×) dry over MgSO4 concentrate to dryness purify via silica gel chromatography (0-50% EtOAc/Hexanes)
来源 ID: ord-e42a8d820ab94b27848eea495bb7a781