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Water → 2-methyl-1-[6-(5-{1-[5-(methylsulfonyl)pyridin-2-yl]-2-(tetrahydro-2H-pyran-4-yl)ethyl}-1H-pyrrol-2-yl)pyridin-3-yl]propane-1,2-diol

HRID 1882068
ノート
印刷プレビュー

反応式

HRID 1882068 の反応式
[CH3:1][C:2]([OH:33])([CH3:32])[CH:3]([C:5]1[CH:6]=[N:7][C:8]([C:11]2[NH:12][C:13]([CH:16]([C:24]3[CH:29]=[CH:28][C:27]([S:30][CH3:31])=[CH:26][N:25]=3)[CH2:17][CH:18]3[CH2:23][CH2:22][O:21][CH2:20][CH2:19]3)=[CH:14][CH:15]=2)=[CH:9][CH:10]=1)[OH:4].[OH2:34].C([O-])([O-])=O.C([O-])([O-])=O.[OH:43]O.OO.OO.[Na+].[Na+].[Na+].[Na+].S([O-])([O-])=O.[Na+].[Na+]>C(#N)C>[CH3:32][C:2]([OH:33])([CH3:1])[CH:3]([C:5]1[CH:6]=[N:7][C:8]([C:11]2[NH:12][C:13]([CH:16]([C:24]3[CH:29]=[CH:28][C:27]([S:30]([CH3:31])(=[O:43])=[O:34])=[CH:26][N:25]=3)[CH2:17][CH:18]3[CH2:19][CH2:20][O:21][CH2:22][CH2:23]3)=[CH:14][CH:15]=2)=[CH:9][CH:10]=1)[OH:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24437Sodium SulfiteHCID 159762Sodium percarbonate2 回HCID 59331498HCID 59331498、化合物

生成物 1

HCID 593312272-methyl-1-[6-(5-{1-[5-(methylsulfonyl)pyridin-2-yl]-2-(tetrahydro-2H-pyran-4-yl)ethyl}-1H-pyrrol-2-yl)pyridin-3-yl]propane-1,2-diol収率 84%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a mixture of 2-methyl-1-[6-(5-{1-[5-(methylsulfanyl)pyridin-2-yl]-2-(tetrahydro-2H-pyran-4-yl)ethyl}-1H-pyrrol-2-yl)pyridin-3-yl]propane-1,2-diol (0.37 g), water (4 mL) and acetonitrile (6 mL) was added sodium percarbonate (0.25 g), and the mixture was stirred at room temperature for 2 hr. To the reaction mixture was added sodium percarbonate (0.10 g), and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added saturated aqueous sodium sulfite solution, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4) and concentrated. The residue was subjected to basic silica gel column chromatography, and the title compound (0.33 g, yield 84%) was obtained as a pale-yellow amorphous solid from a fraction eluted with tetrahydrofuran-hexane (4:1, volume ratio). MS: 500 (MH+).

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe ethyl acetate layer was washed with saturated brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-9fe9a83e06dd496ab0475cd9bcb5bd90
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08318746B2

反応ノート

読み込み中…

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