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Lithium Hydroxide → {4-difluoromethoxy-2-ethyl-8-fluoro-3-[4-(morpholine-4-sulfonyl)benzyl]quinolin-5-yloxy}acetic Acid

HRID 2266601
ノート
印刷プレビュー

反応式

HRID 2266601 の反応式
C[O:2][C:3](=[O:39])[CH2:4][O:5][C:6]1[CH:15]=[CH:14][C:13]([F:16])=[C:12]2[C:7]=1[C:8]([O:35][CH:36]([F:38])[F:37])=[C:9]([CH2:19][C:20]1[CH:25]=[CH:24][C:23]([S:26]([N:29]3[CH2:34][CH2:33][O:32][CH2:31][CH2:30]3)(=[O:28])=[O:27])=[CH:22][CH:21]=1)[C:10]([CH2:17][CH3:18])=[N:11]2.[OH-].[Li+]>O1CCCC1>[F:38][CH:36]([F:37])[O:35][C:8]1[C:7]2[C:12](=[C:13]([F:16])[CH:14]=[CH:15][C:6]=2[O:5][CH2:4][C:3]([OH:39])=[O:2])[N:11]=[C:10]([CH2:17][CH3:18])[C:9]=1[CH2:19][C:20]1[CH:21]=[CH:22][C:23]([S:26]([N:29]2[CH2:30][CH2:31][O:32][CH2:33][CH2:34]2)(=[O:27])=[O:28])=[CH:24][CH:25]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 68781804{4-difluoromethoxy-2-ethyl-8-fluoro-3-[4-(morpholine-4-sulfonyl)benzyl]quinolin-5-yloxy}acetic Acid Methyl Ester

生成物 1

HCID 16660089{4-difluoromethoxy-2-ethyl-8-fluoro-3-[4-(morpholine-4-sulfonyl)benzyl]quinolin-5-yloxy}acetic Acid

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of {4-difluoromethoxy-2-ethyl-8-fluoro-3-[4-(morpholine-4-sulfonyl)benzyl]quinolin-5-yloxy}acetic acid methyl ester (0.16 g), tetrahydrofuran (5.0 mL) and 1.0 M aqueous lithium hydroxide solution (0.32 mL) was stirred at room temperature for 2 hour. The solvent was removed under reduced pressure and the residue was diluted with water. The pH of mixture was adjusted to 4 by the addition of sodium dihydrogenphosphate and extracted with ethyl acetate. The combined extracts were washed with saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was removed under reduced pressure and the residue triturated with a mixture of acetonitrile and water to afford title compound, 0.083 g.

後処理

  1. customThe solvent was removed under reduced pressure
  2. additionthe residue was diluted with water
  3. additionThe pH of mixture was adjusted to 4 by the addition of sodium dihydrogenphosphate
  4. extractionextracted with ethyl acetate
  5. washThe combined extracts were washed with saturated aqueous sodium chloride solution
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customthe residue triturated with a mixture of acetonitrile and water

出典と根拠

ORDレコード
ord-faa1bcfcb6dc4e9ab56ac6a5937a72fe
出典データセット
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07858640B2

反応ノート

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