反应 #1244259

ord-1f5e1383861240a58961321b336c3594

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤The reaction was filtered hot through Celite
  2. 2
    其他The solution was evaporated on a rotary evaporator until crystallization
  3. 3
    温度After cooling in an ice bath
  4. 4
    过滤the crystals were filtered
  5. 5
    洗涤rinsed with Et2O
  6. 6
    其他sucked dry
  7. 7
    其他dried overnight in a vacuum oven at 70° C

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07807340B2uspto-grants-2010_10