反应详情

To a solution of 2-bromomethyl-4-cyano-benzoic acid methyl ester (18.1 g, 71.24 mmol) in THF (300 mL) was added PMBNH2 (23.4 g, 178.1 mmol) at 0° C. and the reaction mixture was stirred at room temperature for 16 hours. After vacuum filtration, the filtrate was concentrated in vacuo. The residue obtained was re-dissolved in EtOAc and washed with water and brine. The organic layer was dried over anhy. Na2SO4, filtered, and concentrated in vacuo to give a crude product which was purified by column chromatography (11.69 g, 56.0%) as a solid.

1. filtrationAfter vacuum filtration
2. concentrationthe filtrate was concentrated in vacuo
3. customThe residue obtained
4. washwashed with water and brine
5. customThe organic layer was dried over anhy
6. filtrationNa2SO4, filtered
7. concentrationconcentrated in vacuo