تفاعل #985264

ord-36b3b88a204247fab995525c4112583e

معادلة التفاعل

COC(=O)c1cc(C(=O)OC)cc([N+](=O)[O-])c1
dimethyl-5-nitroisophthalate
NCCO
ethanolamine
O=C(NCCO)c1cc(C(=O)NCCO)cc([N+](=O)[O-])c1
N,N′-bis(2-hydroxyethyl)-5-nitro-1,3-benzenedicarboxamide
المردود 67.3%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 48 hours
  2. 2
    أخرىThe solvent was removed by evaporation under reduced pressure
  3. 3
    أخرىThe crude product was purified by crystallization from EtOAC

الإجراء التجريبي

A solution containing dimethyl-5-nitroisophthalate (23.9 g, 100 mmol) and ethanolamine (13.4 g, 220 mmol) in methanol (300 mL) was refluxed for 48 hours. The solvent was removed by evaporation under reduced pressure. The crude product was purified by crystallization from EtOAC:MeOH 1 ml v/v) to afford 20.0 g of pure N,N′-bis(2-hydroxyethyl)-5-nitro-1,3-benzenedicarboxamide as white crystals. m.p.=151.3-151.4° C., uncorrected

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07351389B2uspto-grants-2008_04