HRID1066397

反应详情

EQUATION

反应方程式

HRID 1066397 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5,10-dihydrophenazine in an amount of 10 g is dissolved in 100 ml ethanol and added to 2.6 g NaOH dissolved in 2 ml of water. The mixture was heated to reflux and O2 bubbled through for 30 minutes. TLC shows that the 5,10-dihydrophenazine is converted completely to phenazine. The mixture was stripped to a volume of 45 ml and 25 ml water added. After cooling in a refrigerator, 8.0 grams of crude phenazine is collected by filtration. The crude phenazine is dissolved in 80 ml toluene, filtered hot, and stripped to 25 ml. When cooled, 5.86 of still somewhat brown phenazine is collected. After an additional recrystallization from toluene, a further toluene solution (50 ml) is treated with 1.0 g charcoal, reduced to 20 ml, cooled to room temperature and then under refrigeration, to yield 4.0 g (40%) of yellow phenazine.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureto reflux
  3. customO2 bubbled through for 30 minutes
  4. additionadded
  5. temperatureAfter cooling in a refrigerator, 8.0 grams of crude phenazine
  6. filtrationis collected by filtration
  7. dissolutionThe crude phenazine is dissolved in 80 ml toluene
  8. filtrationfiltered hot
  9. temperatureWhen cooled
  10. custom5.86 of still somewhat brown phenazine is collected
  11. customAfter an additional recrystallization from toluene
  12. additiona further toluene solution (50 ml) is treated with 1.0 g charcoal