反応 #985264

ord-36b3b88a204247fab995525c4112583e

反応方程式

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
収率 67.3%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was refluxed for 48 hours
  2. 2
    その他The solvent was removed by evaporation under reduced pressure
  3. 3
    その他The crude product was purified by crystallization from EtOAC

実験手順

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

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07351389B2uspto-grants-2008_04