Acetonitrile → HCID 178503422, 화합물

HRID 394479

반응식

HRID 394479 반응식
[CH3:1][S:2][C:3]1[N:8]=[C:7]([CH:9]2[C:14]([C:15]3[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=3)=[N:13][NH:12][C:11](=[O:25])[CH2:10]2)[CH:6]=[CH:5][N:4]=1.ClC1C(=O)C(C#N)=C(C#N)C(=O)C=1Cl.C(#N)C>CCOCC.CCOC(C)=O>[CH3:1][S:2][C:3]1[N:8]=[C:7]([C:9]2[CH:10]=[C:11]([OH:25])[N:12]=[N:13][C:14]=2[C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([C:21]([F:24])([F:23])[F:22])[CH:16]=2)[CH:6]=[CH:5][N:4]=1

참가 물질

5

반응물 3

HCID 6342AcetonitrileHCID 67752,3-Dichloro-5,6-dicyano-1,4-benzoquinoneHCID 181766265-(2-Methylsulfanylpyrimidin-4-yl)-6-(3-trifluoromethylphenyl)-4,5-dihydro-2H-pyridazin-3-one

생성물 1

HCID 178503422HCID 178503422, 화합물

시약·촉매·용매 1

HCID 21584169Diethylether ethylacetate용매

반응 조건

온도
90 °C

실험 절차

Compound 6 (1.92 g, 5.26 mmol), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (4.78 g, 21.0 mmol), and acetonitrile (30 mL) were combined under argon and heated at 90° C. for 1 h. The solution was cooled and the solvent was removed in vacuo. The crude product was purified by flash column chromatography (methylene chloride:methanol:ammonium hydroxide 95:5:0.5) to give a solid. Trituration with.Et2O EtOAc gave Compound 69: 1.60 g (4.4 mmol, 83%)

후처리

  1. temperatureThe solution was cooled
  2. customthe solvent was removed in vacuo
  3. customThe crude product was purified by flash column chromatography (methylene chloride:methanol:ammonium hydroxide 95:5:0.5)
  4. customto give a solid

출처 및 근거

ORD 기록
ord-97f21f61c67445529680a26e4abcd655
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06602872B1

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