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Propionic Acid → 2-(3-fluoro-4-(hydroxymethyl)phenyl)-N-((1-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methyl)propanamide

HRID 1842877
ノート
印刷プレビュー

反応式

HRID 1842877 の反応式
Cl.[F:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13]([CH2:14][NH2:15])=[CH:12][C:11]([C:16]([F:19])([F:18])[F:17])=[N:10]2)=[CH:5][CH:4]=1.[C:20]([OH:24])(=O)[CH2:21][CH3:22].[CH:25]1[CH:26]=[CH:27][C:28]2N(O)N=N[C:29]=2[CH:30]=1.CN([C:38]([O:42]N1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)[F:53].CCN(C(C)C)C(C)C>C1COCC1.CN(C=O)C.CCOC(C)=O>[F:53][C:29]1[CH:30]=[C:25]([CH:21]([CH3:22])[C:20]([NH:15][CH2:14][C:13]2[N:9]([C:6]3[CH:7]=[CH:8][C:3]([F:2])=[CH:4][CH:5]=3)[N:10]=[C:11]([C:16]([F:17])([F:19])[F:18])[CH:12]=2)=[O:24])[CH:26]=[CH:27][C:28]=1[CH2:38][OH:42]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 1032Propionic AcidHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 70816754(1-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanamine hydrochloride

生成物 1

HCID 70816123
2-(3-fluoro-4-(hydroxymethyl)phenyl)-N-((1-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methyl)propanamide
収率 79.2%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21974620tetrahydrofuran N,N-dimethylformamide溶媒

実験手順

To a stirred solution of (1-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanamine hydrochloride (101 mg, 0.342 mmol, 1.0 eq) in THF/DMF (1/20, v/v, 2.8 mL) was added 2-(3-fluoro-4-hydroxymethyl)phenyl)propionic acid (68 mg, 0.348 mmol, 1.02 equiv.), HOBt (46 mg. 0.342 mmol, 1 equiv.), TBTU (151 mg, 0.342 mmo, 1 equiv.) and DIPEA (0.232 mL, 176 mg, 1.37 mmol, 4 equiv.) and the mixture was stirred for 3 d at room temperature The reaction mixture was diluted with 20 mL of EtOAc and washed with 20 mL of water. The aqueous phase was extracted with EtOAc (3×20 mL), the combined organic phases were dried over magnesium sulfate, evaporated and the residue was purified by column chromatography (EtOAc/cyclohexane (1:1) as eluent) to give 2-(3-fluoro-4-(hydroxymethyl)phenyl)-N-((1-(4-fluorophenyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methyl)propanamide (119 mg, 79%).

後処理

  1. washwashed with 20 mL of water
  2. extractionThe aqueous phase was extracted with EtOAc (3×20 mL)
  3. dry with materialthe combined organic phases were dried over magnesium sulfate
  4. customevaporated
  5. customthe residue was purified by column chromatography (EtOAc/cyclohexane (1:1) as eluent)

出典と根拠

ORDレコード
ord-620ffcd4fe5d4449ba1cc4f131214889
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946204B2

反応ノート

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