Sodium Sulfate → 2,5-Dimethoxy benzoquinone diimine

HRID 653019

반응식

HRID 653019 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([NH2:9])[C:6]([O:10][CH3:11])=[CH:5][C:4]=1[NH2:12].S([O-])([O-])(=O)=O.[Na+].[Na+]>[Ag]=O.C(OC(C)C)(C)C>[CH3:11][O:10][C:6]1[C:7](=[NH:9])[CH:8]=[C:3]([O:2][CH3:1])[C:4](=[NH:12])[CH:5]=1

참가 물질

5

반응물 2

HCID 24436Sodium Sulfate2회HCID 1555944-Amino-2,5-dimethoxyaniline

생성물 1

HCID 539632862,5-Dimethoxy benzoquinone diimine

시약·촉매·용매 2

HCID 92152Silver(II) oxide촉매HCID 7914Diisopropyl Ether용매

실험 절차

0.06 mole (10 g) 2,5-dimethoxy paraphenylene diamine is introduced into a liter of anhydrous isopropyl ether. 21 g silver oxide and 48 g anhydrous sodium sulfate are then added to the same. The resulting mixture is heated at reflux for 6 hours, while maintaining good agitation. After cooling the reaction mixture the sodium sulfate and the silver are filtered out and the filtrate is evaporated to dryness under vacuum. The dry residue which is the above diimine, after recrystallization from a benzene-petroleum ether mixture, yields pure 2,5-dimethoxy benzoquinone diimine having a melting point of 184°.

후처리

  1. temperatureThe resulting mixture is heated
  2. temperatureat reflux for 6 hours
  3. temperaturewhile maintaining good agitation
  4. filtrationthe silver are filtered out
  5. customthe filtrate is evaporated to dryness under vacuum
  6. customafter recrystallization from a benzene-petroleum ether mixture

출처 및 근거

ORD 기록
ord-4457308020e748f0a313bb53c0dad321
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04675130

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