Reacción #1244259

ord-1f5e1383861240a58961321b336c3594

Ecuación de reacción

CCC(C)=O
methyl ethyl ketone
O=C1c2ccccc2C(=O)c2c(O)ccc(O)c21
quinizarin
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOS(=O)(=O)[O-]
ethyl sulfate
CCOc1ccc(OCC)c2c1C(=O)c1ccccc1C2=O
1,4-Diethoxyanthraquinone

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    FiltraciónThe reaction was filtered hot through Celite
  2. 2
    OtroThe solution was evaporated on a rotary evaporator until crystallization
  3. 3
    TemperaturaAfter cooling in an ice bath
  4. 4
    Filtraciónthe crystals were filtered
  5. 5
    Lavadorinsed with Et2O
  6. 6
    Otrosucked dry
  7. 7
    Otrodried overnight in a vacuum oven at 70° C

Procedimiento

A mixture of quinizarin (20.0 g, 83.5 mmol), potassium carbonate (76 g, 550 mmol) and ethyl sulfate (38.6 g, 250 mmol) was refluxed in methyl ethyl ketone (MEK, 950 mL) for 24 hrs. The reaction was filtered hot through Celite using additional hot MEK. The solution was evaporated on a rotary evaporator until crystallization began, then the reaction was allowed to sit overnight. After cooling in an ice bath, the crystals were filtered, rinsed with Et2O, sucked dry, then dried overnight in a vacuum oven at 70° C. The yield was 14.0 g (57%) of yellow/orange crystals.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07807340B2uspto-grants-2010_10