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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
ノート
印刷プレビュー

反応式

HRID 1049490 の反応式
[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]
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 117759958Ethyl 3-(2-(((2-(2-cyano-2-methylpropyl)-2'-fluoro-5'-methoxybiphenyl-4-yl)oxy)methyl)pyridin-4-yl)-3-cyclopropylpropanoate

生成物 1

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

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-7c8de256af2244869c642c603cbf2019
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09382188B2

反応ノート

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