9,10-Phenanthrenedione → 10-(3,5-Dichloro-2-pyridylazo)-9-phenanthrol

HRID 1266920

反応式

HRID 1266920 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.[Cl:17][C:18]1[C:19]([NH:25][NH2:26])=[N:20][CH:21]=[C:22]([Cl:24])[CH:23]=1>C(O)(=O)C>[Cl:17][C:18]1[C:19]([N:25]=[N:26][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])=[N:20][CH:21]=[C:22]([Cl:24])[CH:23]=1

参加物

4

反応物 2

HCID 67639,10-Phenanthrenedione2 回HCID 6009663,5-Dichloro-2-hydrazinylpyridine

生成物 1

HCID 13571850810-(3,5-Dichloro-2-pyridylazo)-9-phenanthrol

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
105 °C

実験手順

Next, a reaction flask was loaded with acetic acid (15 ml) and 9,10-phenanthrenequinone (5.0 g), and the temperature was raised to 105° C. with stirring to dissolve 9,10-phenanthrenequinone. To the resultant, the crystals of 3,5-dichloro-2-hydrazinopyridine (4.6 g) was added in 30 minutes. After stirring at 105 to 110° C. for one hour, the reaction mixture was filtrated. The filtrated crystals were washed with methanol, and then dried to give intended crystals (5.1 g).

後処理

  1. stirringAfter stirring at 105 to 110° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. washThe filtrated crystals were washed with methanol
  4. customdried
  5. customto give

出典と根拠

ORDレコード
ord-5ffcf76dc5404586bdf823c8317970b4
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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