反应 #1244259
ord-1f5e1383861240a58961321b336c3594
反应方程式
methyl ethyl ketone
quinizarin
potassium carbonate
ethyl sulfate
→
1,4-Diethoxyanthraquinone
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1过滤The reaction was filtered hot through Celite
- 2其他The solution was evaporated on a rotary evaporator until crystallization
- 3温度After cooling in an ice bath
- 4过滤the crystals were filtered
- 5洗涤rinsed with Et2O
- 6其他sucked dry
- 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.