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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
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HRID 579388 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-592beed285b84ce1aea36cbe40250baf
출처 데이터셋
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09040717B2

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