Ethanolamine → N~1~,N~3~-Bis(2-hydroxyethyl)-5-nitrobenzene-1,3-dicarboxamide

HRID 898082

반응식

HRID 898082 반응식
CO[C:3](=[O:17])[C:4]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[CH:11]=[C:6]([C:7]([O:9]C)=O)[CH:5]=1.[CH2:18]([CH2:20][NH2:21])[OH:19]>CO>[OH:19][CH2:18][CH2:20][NH:21][C:7]([C:6]1[CH:11]=[C:12]([N+:14]([O-:16])=[O:15])[CH:13]=[C:4]([C:3]([NH:21][CH2:20][CH2:18][OH:19])=[O:17])[CH:5]=1)=[O:9]

참가 물질

4

반응물 2

HCID 700EthanolamineHCID 83316Dimethyl 5-nitroisophthalate

생성물 1

HCID 13140678N~1~,N~3~-Bis(2-hydroxyethyl)-5-nitrobenzene-1,3-dicarboxamide수율 67.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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

후처리

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

출처 및 근거

ORD 기록
ord-36b3b88a204247fab995525c4112583e
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07351389B2

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