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

HRID 1266918

반응식

HRID 1266918 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: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

참가 물질

4

반응물 2

HCID 67639,10-Phenanthrenedione2회HCID 12726913-Chloro-2-hydrazinyl-5-(trifluoromethyl)pyridine

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °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 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).

후처리

  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

출처 및 근거

ORD 기록
ord-d13af6f1ad5747ef991459ec5268d43d
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551682B1

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