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Ethanolamine → 2-chloro-5-beta-aminoethylamino-4-nitro-N-(beta-hydroxyethyl)aniline

HRID 4239
ノート
印刷プレビュー

反応式

HRID 4239 の反応式
[Cl:1][C:2]1[C:11](Cl)=[CH:10][C:5]([NH:6][CH2:7][CH2:8][NH2:9])=[C:4]([N+:13]([O-:15])=[O:14])[CH:3]=1.[CH2:16]([CH2:18][NH2:19])[OH:17]>O>[Cl:1][C:2]1[CH:3]=[C:4]([N+:13]([O-:15])=[O:14])[C:5]([NH:6][CH2:7][CH2:8][NH2:9])=[CH:10][C:11]=1[NH:19][CH2:18][CH2:16][OH:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 700EthanolamineHCID 54360568N-(4,5-dichloro-2-nitrophenyl)ethane-1,2-diamine

生成物 1

HCID 541600842-chloro-5-beta-aminoethylamino-4-nitro-N-(beta-hydroxyethyl)aniline

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

0.04 mole (10 g) of 4,5-dichloro-2-nitro-N-β-aminoethylaniline prepared in the 1st stage is heated in 40 ml of monoethanolamine for 30 minutes to 100° C. The reaction mixture is diluted with 450 ml of iced water. An impurity is precipitated by adding hydrochloric acid and is removed by filtration. The filtrate is made alkaline with concentrated sodium hydroxide solution. The expected product precipitates. After filtration and drying, it is purified as its hydrochloride before being recrystallized from alcohol. It melts at 160° C.

後処理

  1. customAn impurity is precipitated
  2. additionby adding hydrochloric acid
  3. customis removed by filtration
  4. customThe expected product precipitates
  5. filtrationAfter filtration
  6. customdrying
  7. customit is purified as its hydrochloride
  8. custombefore being recrystallized from alcohol

出典と根拠

ORDレコード
ord-4c54e3751d4842d7a5094d5ea6aa2e59
出典データセット
uspto-grants-1988_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04725283

反応ノート

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