Water → HCID 22936659, 화합물

HRID 387962노트

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HRID 387962 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1OS(C(F)(F)F)(=O)=O)[N:9]=[CH:8][CH:7]=[C:6]2[O:21][C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=1.O.[CH3:32][N:33](C)C=O>[C-]#N.[Zn+2].[C-]#N>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[C:32]#[N:33])[N:9]=[CH:8][CH:7]=[C:6]2[O:21][C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-:30])=[O:29])=[CH:24][CH:23]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 6228DimethylformamideHCID 58931114HCID 58931114, 화합물

생성물 1

HCID 22936659HCID 22936659, 화합물

시약·촉매·용매 1

HCID 11186Zinc cyanide (Zn(CN)2)촉매

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온도
110 °C

실험 절차

After dissolving trifluoromethanesulfonic acid 6-methoxy-4-(4-nitrophenoxy)quinolin-7-yl ester (500 mg) in dimethylformamide (5 ml), there were added zinc cyanide (260 mg) and tetrakistriphenylphosphine palladium (0) (130 mg) and the mixture was heated and stirred at 110° C. for 2 hours under a nitrogen stream. Water was added, extraction was performed with ethyl acetate, the organic layer was washed with water and saturated saline in that order and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. Ethyl acetate was used for recrystallization to obtain the title compound (300 mg).

후처리

  1. temperaturethe mixture was heated
  2. extractionextraction
  3. washthe organic layer was washed with water and saturated saline in that order
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customEthyl acetate was used for recrystallization

출처 및 근거

ORD 기록
ord-9a73db7362fa4a86a16e2efd5595b574
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372981B2

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