反应 #3182093
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07582668B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: To a solution of 1,1-dimethylethyl [(1S)-2-(4-bromophenyl)-1-(hydroxymethyl)ethyl]carbamate (70.6 mmol), tripheylphosphine (84.7 mmol), and phthalimide (84.7 mmol) in anhydrous tetrahydrofuran (550 mL) at 0° C. was added dropwise duisopropyl azodicarboxylate (84.7 mmol) over 10 minutes. The reaction continued to stir allowing to warmn to RT over 5 h. The reaction was then concentrated in vacuo and product was triturated out of solution using ethyl acetate (500 mL). The precipitate was filtered, washed with ethyl acetate (3×100 mL), and dried to afford the title product as a white solid (57%). ESMS [M+H]+: 460.4. The reaction was then concentrated in vacuo and product was triturated out of solution The precipitate was filtered washed with ethyl acetate (3×100 mL) dried
来源 ID: ord-f35ae790be8e4ea69de0db49ed78fbbb