9,10-Phenanthrenedione → 10-(3,6-Dimethyl-2-pyrazinylazo)-9-phenanthrol

HRID 1266916

反応式

HRID 1266916 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[C:24]([CH3:25])=[N:23][CH:22]=[C:21]([CH3:26])[N:20]=1)[NH2:18]>C(O)(=O)C>[CH3:25][C:24]1[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])=[N:20][C:21]([CH3:26])=[CH:22][N:23]=1

参加物

4

反応物 2

HCID 67639,10-Phenanthrenedione2 回HCID 15255095HCID 15255095、化合物

生成物 1

HCID 13611639910-(3,6-Dimethyl-2-pyrazinylazo)-9-phenanthrol

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

Next, a reaction flask was loaded with acetic acid (80 ml) and 9,10-phenanthrenequinone (4.0 g), and heated up to 90° C. with stirring to dissolve 9,10-phenanthrenequinone. To the resultant, the crystals of 2-hydrazino-3,6-dimethylpyrazine (2.7 g) was added in 20 minutes. After stirring at 90 to 100° C. for two hours, the reaction mixture was cooled and filtrated. An aqueous solution of sodium hydroxide was added to the filtrate with stirring so that crystals precipitated. The crystals were filtrated and washed with methanol, followed by being recrystallized with dioxane-water. The crystals were then filtrated and dried to give intended crystals (3.3 g).

後処理

  1. stirringAfter stirring at 90 to 100° C. for two hours
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltrated
  4. additionAn aqueous solution of sodium hydroxide was added to the filtrate
  5. stirringwith stirring so that crystals
  6. customprecipitated
  7. filtrationThe crystals were filtrated
  8. washwashed with methanol
  9. customby being recrystallized with dioxane-water
  10. filtrationThe crystals were then filtrated
  11. customdried
  12. customto give

出典と根拠

ORDレコード
ord-22d9b89bb7dd4e698e3b7fa6fb54a52c
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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