反応 #1244259

反応方程式

methyl ethyl ketone

quinizarin

potassium carbonate

ethyl sulfate

→

1,4-Diethoxyanthraquinone

反応条件

後処理

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

実験手順

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.

出典