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

HRID 898082

反応式

HRID 898082 の反応式
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]

参加物

4

反応物 2

HCID 700EthanolamineHCID 83316Dimethyl 5-nitroisophthalate

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

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

後処理

  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

出典と根拠

ORDレコード
ord-36b3b88a204247fab995525c4112583e
出典データセット
uspto-grants-2008_04
特許番号
US07351389B2

関連ノート

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