反応 #52246

ord-5f717293ced543b9a3f0f746b5bde313

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution was heated to 80 C
  2. 2
    workup.STIRRINGstirred for 1 hour
  3. 3
    抽出The product was extracted with methylene chloride
  4. 4
    その他dried
  5. 5
    その他The product was purified by sublimation
  6. 6
    その他yielding white crystals, m.p. 76° C. (44.1 g, 13.45%)

実験手順

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%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855745B2uspto-grants-2005_02