9,10-Phenanthrenedione → 10-[6-(4-Trifluoromethyl-phenoxy)-2-pyridylazo]-9-phenanthrol

HRID 1266923

반응식

HRID 1266923 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.[NH:17]([C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([O:25][C:26]2[CH:31]=[CH:30][C:29]([C:32]([F:35])([F:34])[F:33])=[CH:28][CH:27]=2)[N:20]=1)[NH2:18]>C(O)(=O)C>[F:35][C:32]([F:33])([F:34])[C:29]1[CH:30]=[CH:31][C:26]([O:25][C:21]2[N:20]=[C:19]([N:17]=[N:18][C:13]3[C:14]4[CH:1]=[CH:2][CH:3]=[CH:4][C:5]=4[C:6]4[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=4)[C:12]=3[OH:16])[CH:24]=[CH:23][CH:22]=2)=[CH:27][CH:28]=1

참가 물질

4

반응물 2

HCID 67639,10-Phenanthrenedione2회HCID 185447862-Hydrazino-6-(4-trifluoromethylphenoxy)pyridine

생성물 1

HCID 13571851710-[6-(4-Trifluoromethyl-phenoxy)-2-pyridylazo]-9-phenanthrol

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

Then, a reaction flask was loaded with acetic acid (30 ml) and 9,10-phenanthrenequinone (2.0 g), and the temperature was raised to 100° C. with stirring to dissolve 9,10-phenanthrenequinone. To this mixture, 2-hydrazino-6-(4-trifluoromethylphenoxy)pyridine (3.0 g) was added in 15 minutes. After stirring at 95 to 105° C. for two hours, the reaction mixture was filtrated. The filtrated crystals were successively washed with hot water and hot methanol, followed by recrystallization with dioxane-water to give crystals, which were then filtrated and dried to give intended crystals (3.5 g).

후처리

  1. stirringAfter stirring at 95 to 105° C. for two hours
  2. filtrationthe reaction mixture was filtrated
  3. washThe filtrated crystals were successively washed with hot water and hot methanol
  4. customfollowed by recrystallization with dioxane-water
  5. customto give crystals, which
  6. filtrationwere then filtrated
  7. customdried
  8. customto give

출처 및 근거

ORD 기록
ord-f214a62caa804413ae27f261d2a384c1
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06551682B1

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