9,10-Phenanthrenedione → 10-[3-Chloro-5-(trifluoro-methyl)-2-pyridylazo]-9-phenanthrol

HRID 1266918

反応式

HRID 1266918 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:28][NH2:29])=[N:20][CH:21]=[C:22]([C:24]([F:27])([F:26])[F:25])[CH:23]=1>C(O)(=O)C>[Cl:17][C:18]1[C:19]([N:28]=[N:29][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]([C:24]([F:27])([F:25])[F:26])[CH:23]=1

参加物

4

反応物 2

HCID 67639,10-Phenanthrenedione2 回HCID 12726913-Chloro-2-hydrazinyl-5-(trifluoromethyl)pyridine

生成物 1

HCID 13571851310-[3-Chloro-5-(trifluoro-methyl)-2-pyridylazo]-9-phenanthrol

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
100 °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 100° C. with stirring to dissolve 9,10-phenanthrenequinone. To the resultant, the crystals of 3-chloro-2-hydrazino-5-(trifluoromethyl)-pyridine (5.0 g) was added in 30 minutes. After stirring at 100 to 105° C. for one hour, the reaction mixture was filtrated. After being washed with methanol, the obtained crystals were dried to give intended crystals (5.6 g).

後処理

  1. stirringAfter stirring at 100 to 105° C. for one hour
  2. filtrationthe reaction mixture was filtrated
  3. washAfter being washed with methanol
  4. customthe obtained crystals were dried
  5. customto give

出典と根拠

ORDレコード
ord-d13af6f1ad5747ef991459ec5268d43d
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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