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

HRID 1266920

반응식

HRID 1266920 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.[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

참가 물질

4

반응물 2

HCID 67639,10-Phenanthrenedione2회HCID 6009663,5-Dichloro-2-hydrazinylpyridine

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
105 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5ffcf76dc5404586bdf823c8317970b4
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551682B1

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