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Hydrochloric Acid → 2-{4-[(9R)-9-Hydroxy-2-(3-hydroxy-3-methylbutyloxy)-9-(trifluoromethyl)-9H-fluoren-4-yl]-1H-pyrazol-1-yl}-2-methylpropionic acid

HRID 579388
ノート
印刷プレビュー

反応式

HRID 579388 の反応式
[OH:1][C@@:2]1([C:35]([F:38])([F:37])[F:36])[C:14]2[CH:13]=[C:12]([O:15][CH2:16][CH2:17][C:18]([OH:21])([CH3:20])[CH3:19])[CH:11]=[C:10]([C:22]3[CH:23]=[N:24][N:25]([C:27]([CH3:34])([CH3:33])[C:28]([O:30]CC)=[O:29])[CH:26]=3)[C:9]=2[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2.[OH-].[Na+].Cl>C(O)C>[OH:1][C@@:2]1([C:35]([F:37])([F:38])[F:36])[C:14]2[CH:13]=[C:12]([O:15][CH2:16][CH2:17][C:18]([OH:21])([CH3:19])[CH3:20])[CH:11]=[C:10]([C:22]3[CH:23]=[N:24][N:25]([C:27]([CH3:33])([CH3:34])[C:28]([OH:30])=[O:29])[CH:26]=3)[C:9]=2[C:8]2[C:3]1=[CH:4][CH:5]=[CH:6][CH:7]=2
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 117599404Ethyl 2-{4-[(9R)-9-hydroxy-2-(3-hydroxy-3-methylbutyloxy)-9-(trifluoromethyl)-9H-fluoren-4-yl]-1H-pyrazol-1-yl}-2-methylpropionate

生成物 1

HCID 1175992732-{4-[(9R)-9-Hydroxy-2-(3-hydroxy-3-methylbutyloxy)-9-(trifluoromethyl)-9H-fluoren-4-yl]-1H-pyrazol-1-yl}-2-methylpropionic acid収率 108%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

Ethyl 2-{4-[(9R)-9-hydroxy-2-(3-hydroxy-3-methylbutyloxy)-9-(trifluoromethyl)-9H-fluoren-4-yl]-1H-pyrazol-1-yl}-2-methylpropionate (68.4 g) was dissolved in ethanol (256 ml), 4N aqueous sodium hydroxide (128 ml) was added, and the mixture was stirred at room temperature for 2.5 hr. The reaction mixture was ice-cooled, 2N hydrochloric acid (333 ml) was added dropwise, and the mixture was extracted with ethyl acetate (500 ml). The obtained organic layer was washed successively with water (400 ml, twice) and saturated brine (400 ml). The obtained organic layer was dried over anhydrous sodium sulfate, the insoluble material was filtered off, and the solvent in the filtrate was evaporated to give the title compound (70.0 g).

後処理

  1. temperaturecooled
  2. extractionthe mixture was extracted with ethyl acetate (500 ml)
  3. washThe obtained organic layer was washed successively with water (400 ml
  4. dry with materialThe obtained organic layer was dried over anhydrous sodium sulfate
  5. filtrationthe insoluble material was filtered off
  6. customthe solvent in the filtrate was evaporated

出典と根拠

ORDレコード
ord-592beed285b84ce1aea36cbe40250baf
出典データセット
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09040717B2

反応ノート

読み込み中…

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