反应详情

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.

1. concentrationThe reaction was then concentrated in vacuo and product
2. customwas triturated out of solution
3. filtrationThe precipitate was filtered
4. washwashed with ethyl acetate (3×100 mL)
5. customdried