تفاعل #1244259

ord-1f5e1383861240a58961321b336c3594

معادلة التفاعل

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

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحThe reaction was filtered hot through Celite
  2. 2
    أخرىThe solution was evaporated on a rotary evaporator until crystallization
  3. 3
    درجة الحرارةAfter cooling in an ice bath
  4. 4
    ترشيحthe crystals were filtered
  5. 5
    غسيلrinsed with Et2O
  6. 6
    أخرىsucked dry
  7. 7
    أخرىdried overnight in a vacuum oven at 70° C

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07807340B2uspto-grants-2010_10