반응 #470378

ord-f1acf67d1cd44f2980ceb3ef2322c62b

반응 방정식

COC(=O)Cl
Methylchloroformate
O=C1C=CC(=O)N1
maleimide
CN1CCOCC1
NMM
COC(=O)N1C(=O)C=CC1=O
product
수율 55.0%
COC(=O)N1C(=O)C=CC1=O
N-(Methoxycarbonyl)maleimide
수율 55.0%

시약

없음

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered
  2. 2
    세척washed with EtOAc
  3. 3
    세척washed with cold water
  4. 4
    건조dried over anhydrous Na2SO4
  5. 5
    여과After filtration and evaporation under vacuum a pink solid
  6. 6
    기타was obtained
  7. 7
    기타Purification by column chromatography on silica gel (Hexane-EtOAc, 1:1

실험 절차

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%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08367065B2uspto-grants-2013_02