반응 #52246

ord-5f717293ced543b9a3f0f746b5bde313

반응 방정식

O=C([O-])[O-].[K+].[K+]
K2CO3
O=C1C=CC(=O)O1
Maleic anhydride
NCCO
ethanolamine
CC(=O)OC(C)=O
acetic anhydride
CC(=O)[O-].[Na+]
sodium acetate
CC(=O)OCCC1=CC(=O)NC1=O
Acetoxy Ethyl Maleimide

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution was heated to 80 C
  2. 2
    workup.STIRRINGstirred for 1 hour
  3. 3
    추출The product was extracted with methylene chloride
  4. 4
    기타dried
  5. 5
    기타The product was purified by sublimation
  6. 6
    기타yielding white crystals, m.p. 76° C. (44.1 g, 13.45%)

실험 절차

Maleic anhydride (172.32 g, 1.75 mol) was added to ethanolamine (107.34 g, 1.75 mol) and dissolved in 500 mL of acetone while stirring overnight in an ice bath. To the solution, 400 mL of acetic anhydride (4.23 mol) was added with sodium acetate (144 g, 1.75 mol). The solution was heated to 80 C and stirred for 1 hour. The contents were poured into ice water and the acetic acid neutralized with K2CO3. The product was extracted with methylene chloride and then dried using magnesium sulfate. The product was purified by sublimation yielding white crystals, m.p. 76° C. (44.1 g, 13.45%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06855745B2uspto-grants-2005_02