反应详情

温度

0 °C

Methylchloroformate (4.4 mL, 56.7 mmol, 1 eq) was added to a solution of maleimide (5.5 g, 56.7 mmol, 1 eq) and NMM (6.2 mL, 56.7 mmol, 1 eq) in 200 mL of EtOAc at 0° C. The suspension was stirred at 0° C. for 30 minutes, filtered and washed with EtOAc. Filtrate and washings were combined and washed with cold water and dried over anhydrous Na2SO4. After filtration and evaporation under vacuum a pink solid was obtained. Purification by column chromatography on silica gel (Hexane-EtOAc, 1:1, v/v) provided the product (4.8 g, 55%).

1. filtrationfiltered
2. washwashed with EtOAc
3. washwashed with cold water
4. dry with materialdried over anhydrous Na2SO4
5. filtrationAfter filtration and evaporation under vacuum a pink solid
6. customwas obtained
7. customPurification by column chromatography on silica gel (Hexane-EtOAc, 1:1