Hydrazine hydrate (1:1) → HCID 20096580、化合物

HRID 1769975ノート

反応式

HRID 1769975 の反応式
O.NN.[CH2:4]([O:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([N:16]2C(=O)C3=CC=CC=C3C2=O)=[CH:12][C:11]=1[N+:27]([O-:29])=[O:28])=[O:8])[CH3:5]>COCCOC>[NH2:16][C:13]1[CH:14]=[CH:15][C:10]([NH:9][C:7]([O:6][CH2:4][CH3:5])=[O:8])=[C:11]([N+:27]([O-:29])=[O:28])[CH:12]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 20096586HCID 20096586、化合物

生成物 1

HCID 20096580HCID 20096580、化合物収率 93.7%

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

実験手順

21.0 g (0.42 mol) hydrazine hydrate is added dropwise with stirring under reflux to a suspension of 142.1 g (0.4 mol) 2-ethoxycarbonylamino-5-phthalimido-nitrobenzene in 700 ml 1,2-dimethoxyethane and the mixture is allowed to react for a further 2 hours. After cooling to room temperature, precipitated phthalyl hydrazide is filtered off and the dark red filtrate in the vacuum is evaporated to dryness. The remaining solid residue is recrystallized from about 150 ml toluene. 84.4 g 5-amino-2-ethoxycarbonylaminonitrobenzene are obtained as dark red crystals.

後処理

  1. customto react for a further 2 hours
  2. customprecipitated phthalyl hydrazide
  3. filtrationis filtered off
  4. customthe dark red filtrate in the vacuum is evaporated to dryness
  5. customThe remaining solid residue is recrystallized from about 150 ml toluene

出典と根拠

ORDレコード
ord-45b80b347353493b8e33c6cd48395418
出典データセット
uspto-grants-1995_01
特許番号
US05384330

反応ノート

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