Hydrazine hydrate (1:1) → HCID 20096580, 화합물

HRID 1769975노트

반응식

HRID 1769975 반응식
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

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 20096586HCID 20096586, 화합물

생성물 1

HCID 20096580HCID 20096580, 화합물수율 93.7%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-45b80b347353493b8e33c6cd48395418
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05384330

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