Sodium Hydroxide → HCID 22281907, 화합물

HRID 397277노트

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HRID 397277 반응식
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

참가 물질

4

반응물 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

생성물 1

HCID 22281907HCID 22281907, 화합물수율 82.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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 14) (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)

후처리

  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

출처 및 근거

ORD 기록
ord-ee1111db13214b159a2adfc494df81c2
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610518B2

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