Sodium Sulfate → 2,5-Dimethoxy benzoquinone diimine

HRID 653019

反応式

HRID 653019 の反応式
[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

参加物

5

反応物 2

HCID 24436Sodium Sulfate2 回HCID 1555944-Amino-2,5-dimethoxyaniline

生成物 1

HCID 539632862,5-Dimethoxy benzoquinone diimine

試薬・触媒・溶媒 2

HCID 92152Silver(II) oxide触媒HCID 7914Diisopropyl Ether溶媒

実験手順

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°.

後処理

  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

出典と根拠

ORDレコード
ord-4457308020e748f0a313bb53c0dad321
出典データセット
uspto-grants-1987_06
特許番号
US04675130

関連ノート

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