반응 #1244259

ord-1f5e1383861240a58961321b336c3594

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The reaction was filtered hot through Celite
  2. 2
    기타The solution was evaporated on a rotary evaporator until crystallization
  3. 3
    온도After cooling in an ice bath
  4. 4
    여과the crystals were filtered
  5. 5
    세척rinsed with Et2O
  6. 6
    기타sucked dry
  7. 7
    기타dried overnight in a vacuum oven at 70° C

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07807340B2uspto-grants-2010_10