反应 #985264

ord-36b3b88a204247fab995525c4112583e

反应方程式

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
收率 67.3%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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

来源

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