反应 #3690723
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06747016B1
反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a suspension of 7.73 g (50 mmol) of 6-chloropurine in 350 ml of absolute THF were added 14.43 g (55 mmol) triphenylphosphine at −10 to 0° C. followed by 9.57 g (55 mmol) of diethyl azodicarboxylate and 14.8 g (50 mmol) of N-benzyloxycarbonyl-L-serine tert-butyl ester in 100 ml of absolute THF, and the mixture was stirred at 0° C. for 48 h. The solvent was evaporated, the residue was dissolved in EE/heptane (2:1), filtered and the solvent was removed in vacuo. The crude product was purified by flash chromatography on silica gel (EE/n-heptane (1:1) and DCM/EE (85:15)). Yield: 6.6 g. The solvent was evaporated the residue was dissolved in EE/heptane (2:1) filtered the solvent was removed in vacuo The crude product was purified by flash chromatography on silica gel (EE/n-heptane (1:1) and DCM/EE (85:15))
来源 ID: ord-822b8fc58d8144c9805545109c5f6d27