반응 #1244259
ord-1f5e1383861240a58961321b336c3594
반응 방정식
methyl ethyl ketone
quinizarin
potassium carbonate
ethyl sulfate
→
1,4-Diethoxyanthraquinone
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과The reaction was filtered hot through Celite
- 2기타The solution was evaporated on a rotary evaporator until crystallization
- 3온도After cooling in an ice bath
- 4여과the crystals were filtered
- 5세척rinsed with Et2O
- 6기타sucked dry
- 7기타dried 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.