9,10-Phenanthrenedione → 10-[6-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2-pyridylazo]-9-phenanthrol

HRID 1266926

반응식

HRID 1266926 반응식
[CH:1]1[C:14]2[C:13](=O)[C:12](=[O:16])[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[NH:17]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][CH2:26][C:27]([F:38])([F:37])[C:28]([F:36])([F:35])[C:29]([F:34])([F:33])[CH:30]([F:32])[F:31])[N:20]=1)[NH2:18]>C(O)(=O)C>[F:38][C:27]([F:37])([C:28]([F:35])([F:36])[C:29]([F:33])([F:34])[CH:30]([F:32])[F:31])[CH2:26][O:25][C:21]1[N:20]=[C:19]([N:17]=[N:18][C:13]2[C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=3[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:12]=2[OH:16])[CH:24]=[CH:23][CH:22]=1

참가 물질

4

반응물 2

HCID 67639,10-Phenanthrenedione2회HCID 185447822-Hydrazino-6-(2,2,3,3,4,4,5,5-octafluoropentyloxy)pyridine

생성물 1

HCID 13638834310-[6-(2,2,3,3,4,4,5,5-Octafluoropentyloxy)-2-pyridylazo]-9-phenanthrol

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
110 °C

실험 절차

Next, a reaction flask was loaded with acetic acid (54 ml) and 9,10-phenanthrenequinone (3.8 g), and the temperature was raised to 110° C. with stirring to dissolve 9,10-phenanthrenequinone. To this mixture, 2-hydrazino-6-(2,2,3,3,4,4,5,5-octafluoropentyloxy)pyridine (10 g) was added in 30 minutes. After stirring at 110° C. for one hour, the reaction mixture was filtrated. Crystals were stirred in methanol (100 ml) for 30 minutes, filtrated and dried to give intended crystals (5.2 g).

후처리

  1. stirringAfter stirring at 110° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. stirringCrystals were stirred in methanol (100 ml) for 30 minutes
  4. filtrationfiltrated
  5. customdried
  6. customto give

출처 및 근거

ORD 기록
ord-65e0b6deb2c2449c93641d4701329184
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551682B1

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