تفاعل #52246

ord-5f717293ced543b9a3f0f746b5bde313

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe solution was heated to 80 C
  2. 2
    workup.STIRRINGstirred for 1 hour
  3. 3
    استخلاصThe product was extracted with methylene chloride
  4. 4
    أخرىdried
  5. 5
    أخرىThe product was purified by sublimation
  6. 6
    أخرىyielding white crystals, m.p. 76° C. (44.1 g, 13.45%)

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06855745B2uspto-grants-2005_02