Monoperoxyphthalic Acid Magnesium Salt → 8-{3-[1-(4-Chloro-phenyl)-2-(1-oxy-pyridin-4-yl)-ethyl]-phenyl}-6-isopropyl-quinoline

HRID 896685ノート

反応式

HRID 896685 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:16]2[CH:17]=[C:18]([C:22]3[CH:23]=[C:24]([CH:32]([CH3:34])[CH3:33])[CH:25]=[C:26]4[C:31]=3[N:30]=[CH:29][CH:28]=[CH:27]4)[CH:19]=[CH:20][CH:21]=2)[CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=[CH:4][CH:3]=1.C1C=C(C([O-])=[O:42])C(C(O[O-])=O)=CC=1.[Mg+2]>C(Cl)Cl.CO.C(=O)(O)[O-].[Na+].C(OCC)(=O)C>[CH3:33][CH:32]([C:24]1[CH:25]=[C:26]2[CH:27]=[CH:28][CH:29]=[N:30][C:31]2=[C:22]([C:18]2[CH:19]=[CH:20][CH:21]=[C:16]([CH:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)[CH2:9][C:10]3[CH:11]=[CH:12][N+:13]([O-:42])=[CH:14][CH:15]=3)[CH:17]=2)[CH:23]=1)[CH3:34]

参加物

6

反応物 2

HCID 10130449Monoperoxyphthalic Acid Magnesium SaltHCID 101831968-(3-(1-(4-Chlorophenyl)-2-(pyridin-4-yl)ethyl)phenyl)-6-isopropylquinoline

生成物 1

HCID 102059788-{3-[1-(4-Chloro-phenyl)-2-(1-oxy-pyridin-4-yl)-ethyl]-phenyl}-6-isopropyl-quinoline

試薬・触媒・溶媒 3

HCID 8857Ethyl Acetate溶媒HCID 516892Sodium Bicarbonate溶媒HCID 21226129Dichloromethane methanol溶媒

実験手順

To a solution of Example 60 (100 mg, 0.22 mmol) in CH2Cl2/MeOH (1:1, 6 mL) was added MMPP (320 mg, 0.65 mmol). After 18 h, the resulting reaction mixture was diluted with a sodium bicarbonate solution and ethyl acetate. The organic extracts were washed (H2O, brine), dried (MgSO4), filtered and concentrated. Purification by flash chromatography (eluting with ethanol/ethyl acetate, 10:90 to 25:75) provided the title compound.

後処理

  1. customthe resulting reaction mixture
  2. washThe organic extracts were washed (H2O, brine)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification
  7. washby flash chromatography (eluting with ethanol/ethyl acetate, 10:90 to 25:75)

出典と根拠

ORDレコード
ord-c0af372188c1414f9ec337d53316ca98
出典データセット
uspto-grants-2005_07
特許番号
US06919353B2

反応ノート

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