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Hydrochloric Acid → 3-(2-(((2-(2-Cyano-2-methylpropyl)-2'-fluoro-5'-methoxybiphenyl-4-yl)oxy)methyl)pyridin-4-yl)-3-cyclopropylpropanoic acid

HRID 1049490
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HRID 1049490 반응식
[C:1]([C:3]([CH3:39])([CH3:38])[CH2:4][C:5]1[CH:10]=[C:9]([O:11][CH2:12][C:13]2[CH:18]=[C:17]([CH:19]([CH:26]3[CH2:28][CH2:27]3)[CH2:20][C:21]([O:23]CC)=[O:22])[CH:16]=[CH:15][N:14]=2)[CH:8]=[CH:7][C:6]=1[C:29]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[CH:31][C:30]=1[F:37])#[N:2].[OH-].[Na+].Cl>C(O)C>[C:1]([C:3]([CH3:39])([CH3:38])[CH2:4][C:5]1[CH:10]=[C:9]([O:11][CH2:12][C:13]2[CH:18]=[C:17]([CH:19]([CH:26]3[CH2:27][CH2:28]3)[CH2:20][C:21]([OH:23])=[O:22])[CH:16]=[CH:15][N:14]=2)[CH:8]=[CH:7][C:6]=1[C:29]1[CH:34]=[C:33]([O:35][CH3:36])[CH:32]=[CH:31][C:30]=1[F:37])#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 117759958Ethyl 3-(2-(((2-(2-cyano-2-methylpropyl)-2'-fluoro-5'-methoxybiphenyl-4-yl)oxy)methyl)pyridin-4-yl)-3-cyclopropylpropanoate

생성물 1

HCID 1177600393-(2-(((2-(2-Cyano-2-methylpropyl)-2'-fluoro-5'-methoxybiphenyl-4-yl)oxy)methyl)pyridin-4-yl)-3-cyclopropylpropanoic acid수율 99.3%

시약·촉매·용매 1

HCID 702
Ethanol
용매

실험 절차

To a solution of ethyl 3-(2-(((2-(2-cyano-2-methylpropyl)-2′-fluoro-5′-methoxybiphenyl-4-yl)oxy)methyl)pyridin-4-yl)-3-cyclopropylpropanoate (234 mg) in ethanol (5.0 mL) was added 2N aqueous sodium hydroxide solution (0.44 mL), and the mixture was stirred at room temperature for 16 hr. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (220 mg) as a white solid.

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-7c8de256af2244869c642c603cbf2019
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09382188B2

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