Hydrogen Peroxide → N-Anthraquinon-1-ylacetamide

HRID 461399

反応式

HRID 461399 の反応式
[NH:1]([C:5]1[C:18]2[CH2:17][C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:19])[C:9]=2[CH:8]=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3].[O-:20][Si]([O-])=O.[Na+].[Na+].OO>O>[NH:1]([C:5]1[C:18]2[C:17](=[O:20])[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10](=[O:19])[C:9]=2[CH:8]=[CH:7][CH:6]=1)[C:2]([CH3:4])=[O:3]

参加物

5

反応物 3

HCID 784Hydrogen Peroxide2 回HCID 23266Sodium SilicateHCID 213936134-Acetamino-anthrone

生成物 1

HCID 76760N-Anthraquinon-1-ylacetamide収率 94.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

125.5 g (0.5 mole) of 4-acetamino-anthrone in 1.5 liters of water are warmed to 70°. 50 ml of sodium water glass are added (d = 1.35) and 400 ml of a hydrogen peroxide solution which contains 80 g of H2O2 per liter are then allowed to run in dropwise in the course of 1 hour. Appropriately, a slight stream of nitrogen is passed over the surface during the reaction. The mixture is then stirred at between 70° and 90° C until no further starting material is found in a sample which is withdrawn and examined by thin layer chromatography. In the course of the oxidation, the suspension has developed an intense yellow color. The suspension is filtered and the product washed until neutral. After drying, 125 g of 1-acetamino-anthraquinone with a melting point of 221° C are obtained.

後処理

  1. customdropwise in the course of 1 hour
  2. customAppropriately, a slight stream of nitrogen is passed over the surface during the reaction
  3. customis withdrawn
  4. filtrationThe suspension is filtered
  5. washthe product washed until neutral
  6. customAfter drying

出典と根拠

ORDレコード
ord-2b5037d0ab4c47f2852d2fe302e8849a
出典データセット
uspto-grants-1977_12
特許番号
US04062875

関連ノート

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