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

HRID 1266926

反応式

HRID 1266926 の反応式
[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

参加物

4

反応物 2

HCID 67639,10-Phenanthrenedione2 回HCID 185447822-Hydrazino-6-(2,2,3,3,4,4,5,5-octafluoropentyloxy)pyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
110 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-65e0b6deb2c2449c93641d4701329184
出典データセット
uspto-grants-2003_04
特許番号
US06551682B1

関連ノート

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