Sodium Hydroxide → HCID 22281907、化合物

HRID 1368666ノート

反応式

HRID 1368666 の反応式
C([O:4][CH2:5][CH2:6][O:7][C:8]1[C:12]([C:13]2[CH:21]=[CH:20][C:16]3[O:17][CH2:18][O:19][C:15]=3[CH:14]=2)=[C:11]([N:22](S(C2C=CC(C(C)C)=CN=2)(=O)=O)[S:23]([C:26]2[CH:31]=[CH:30][C:29]([CH:32]([CH3:34])[CH3:33])=[CH:28][N:27]=2)(=[O:25])=[O:24])[N:10]([CH3:47])[N:9]=1)(=O)C.[OH-].[Na+]>C(O)C>[O:17]1[C:16]2[CH:20]=[CH:21][C:13]([C:12]3[C:8]([O:7][CH2:6][CH2:5][OH:4])=[N:9][N:10]([CH3:47])[C:11]=3[NH:22][S:23]([C:26]3[CH:31]=[CH:30][C:29]([CH:32]([CH3:34])[CH3:33])=[CH:28][N:27]=3)(=[O:25])=[O:24])=[CH:14][C:15]=2[O:19][CH2:18]1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 222819602-[(4-(1,3-benzodioxol-5-yl)-5-{bis[(5-isopropyl-2-pyridinyl)sulfonyl]amino}-1-methyl-1H-pyrazol-3-yl)oxy]ethyl acetate

生成物 1

HCID 22281907HCID 22281907、化合物収率 82.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 2-[(4-(1,3-benzodioxol-5-yl)-5-{bis[(5-isopropyl-2-pyridinyl)sulfonyl]amino}-1-methyl-1H-pyrazol-3-yl)oxy]ethyl acetate (Preparation 67) (9.0 g) in ethanol (200 ml) was added 2.0M aqueous sodium hydroxide (25 ml). The reaction was stirred for 30 min and concentrated under reduced pressure and the residue was poured onto 0.5M aqueous citric acid (300 ml). This was extracted with ethyl acetate (3×80 ml) and dried over magnesium sulfate. The solvent was removed under reduced pressure and the crude residue was purified by silica (230 g) chromatography eluting with a gradient of 50% ethyl acetate in hexane to 70% ethyl acetate in hexane to afford the title product as a white solid (5.0 g)

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionthe residue was poured onto 0.5M aqueous citric acid (300 ml)
  3. extractionThis was extracted with ethyl acetate (3×80 ml)
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customthe crude residue was purified by silica (230 g) chromatography
  7. washeluting with a gradient of 50% ethyl acetate in hexane to 70% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-75cc63df5ba84be29ef7771812ec042f
出典データセット
uspto-grants-2003_06
特許番号
US06573270B1

反応ノート

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