反应 #1895539
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08324179B2
反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Compound 35.7 (2.2 g, 9.32 mmol) was dissolved in 10 mL ethyleneglycol, and then treated with NaF (2.2 g), KHF2 (2.2 g). The mixture was stirred at 200° C. for 4 h, cooled to r.t. and then treated with water (150 mL). The aqueous mixture was extracted twice with 200 mL EtOAc. The organic extracts were combined, dried over MgSO4, filtered and concentrated down under reduced pressure. The residue was subjected to a silica gel column chromatography eluting with 20-100% EtOAc in hexane to give compound 35.8 (786 mg, 33% yield). cooled to r.t. The aqueous mixture was extracted twice with 200 mL EtOAc dried over MgSO4 filtered concentrated down under reduced pressure eluting with 20-100% EtOAc in hexane
来源 ID: ord-20c1a4c8c9ed4e1398160e656d798f82