反应 #1267942
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US09206191B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A mixture of tert-butyl(3-hydroxycyclopentyl)carbamate (800 mg, 3.98 mmol) and Dess-martin reagent (3.6 g, 8.15 mmol) in DCM (20 mL) was stirred at RT overnight. And then, the reaction was quenched by addition of sat. aqueous solution of NaHCO3 and sat. aqueous solution of Na2SO3. The resulting mixture was extracted with DCM (20 mL×3). The combined organic layers were dried over Na2SO4, and then concentrated in vacuo. The residue was purified by silica-gel chromatography to afford tert-butyl(3-oxocyclopentyl)carbamate as a white solid (730 mg). And then, the reaction was quenched by addition of sat. aqueous solution of NaHCO3 and sat. aqueous solution of Na2SO3 The resulting mixture was extracted with DCM (20 mL×3) The combined organic layers were dried over Na2SO4 concentrated in vacuo The residue was purified by silica-gel chromatography
来源 ID: ord-97abb1b1c9a84484810a380806095b77