Sodium Hydroxide → Phenazine

HRID 1066397

반응식

HRID 1066397 반응식
[CH:1]1[C:14]2[NH:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[NH:6][C:5]=2[CH:4]=[CH:3][CH:2]=1.[OH-].[Na+]>C(O)C.O>[CH:11]1[C:12]2[C:7](=[N:6][C:5]3[C:14]([N:13]=2)=[CH:1][CH:2]=[CH:3][CH:4]=3)[CH:8]=[CH:9][CH:10]=1

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 3453305,10-Dihydrophenazine

생성물 1

HCID 4757Phenazine수율 40%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-14c5d55802f541edae17991608e8d66d
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06242602B1

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