Реакция #1244259

Уравнение реакции

methyl ethyl ketone

quinizarin

potassium carbonate

ethyl sulfate

→

1,4-Diethoxyanthraquinone

Условия реакции

Обработка

1. 1
   ФильтрацияThe reaction was filtered hot through Celite
2. 2
   ДругоеThe solution was evaporated on a rotary evaporator until crystallization
3. 3
   ТемператураAfter cooling in an ice bath
4. 4
   Фильтрацияthe crystals were filtered
5. 5
   Промывкаrinsed with Et2O
6. 6
   Другоеsucked dry
7. 7
   Другоеdried overnight in a vacuum oven at 70° C

Методика

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.

Источник