Реакция #470378

Уравнение реакции

Methylchloroformate

maleimide

NMM

→

product

Выход 55.0%

N-(Methoxycarbonyl)maleimide

Выход 55.0%

Растворители

EtOAc

Условия реакции

Обработка

1. 1
   Фильтрацияfiltered
2. 2
   Промывкаwashed with EtOAc
3. 3
   Промывкаwashed with cold water
4. 4
   Сушкаdried over anhydrous Na2SO4
5. 5
   ФильтрацияAfter filtration and evaporation under vacuum a pink solid
6. 6
   Другоеwas obtained
7. 7
   ДругоеPurification by column chromatography on silica gel (Hexane-EtOAc, 1:1

Методика

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%).

Источник