Реакция #548581

ord-2b5037d0ab4c47f2852d2fe302e8849a

Уравнение реакции

OO
H2O2
O=[Si]([O-])[O-].[Na+].[Na+]
sodium water glass
OO
hydrogen peroxide
CC(=O)Nc1cccc2c1Cc1ccccc1C2=O
4-acetamino-anthrone
CC(=O)Nc1cccc2c1C(=O)c1ccccc1C2=O
1-acetamino-anthraquinone
Выход 94.3%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеdropwise in the course of 1 hour
  2. 2
    ДругоеAppropriately, a slight stream of nitrogen is passed over the surface during the reaction
  3. 3
    Другоеis withdrawn
  4. 4
    ФильтрацияThe suspension is filtered
  5. 5
    Промывкаthe product washed until neutral
  6. 6
    ДругоеAfter drying

Методика

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 The mixture is then stirred at between 70° and 90° C until no further starting material is found in a sample which is withdrawn and examined by thin layer chromatography.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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04062875uspto-grants-1977_12