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1-Bromo-3-chloropropane → 1-(1-(3-chloropropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one

HRID 2390444
ノート
印刷プレビュー

反応式

HRID 2390444 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([N:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=4)=[CH:12][C:11]3=[O:26])=[CH:7][CH:8]=2)[CH:3]=[N:2]1.Br[CH2:28][CH2:29][CH2:30][Cl:31].C([O-])([O-])=O.[Cs+].[Cs+]>CS(C)=O.O>[Cl:31][CH2:30][CH2:29][CH2:28][N:1]1[C:9]2[C:4](=[CH:5][C:6]([N:10]3[CH:15]=[CH:14][C:13]([C:16]4[CH:21]=[CH:20][C:19]([C:22]([F:24])([F:25])[F:23])=[CH:18][CH:17]=4)=[CH:12][C:11]3=[O:26])=[CH:7][CH:8]=2)[CH:3]=[N:2]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 80061-Bromo-3-chloropropaneHCID 10796Cesium carbonateHCID 576255401-(1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one

生成物 1

HCID 667191041-(1-(3-chloropropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒

実験手順

To a solution of 1-(1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one (278 mg, 0.783 mmol) in DMSO (4.0 mL) was added 3-bromo-1-chloropropane (1.23 g, 7.83 mmol) and Cs2CO3 (765 mg, 2.35 mmol), and the reaction was stirred at ambient temperature for 18 h. The reaction was diluted with H2O (25 mL) and extracted with EtOAc (3×25 mL). The extracts were washed with brine (25 mL), dried over Na2SO4, and concentrated. Flash chromatography (silica gel, CH2Cl2/MeOH, 100:1) yielded 1-(1-(3-chloropropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one. To a solution of 1-(1-(3-chloropropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one (84 g, 0.20 mmol) in DMF (1.5 mL) was added potassium phthalimide (41 mg, 0.22 mmol) and the reaction was heated to 100° C. for 4 h. The reaction was allowed to cool, diluted with H2O (20 mL) and extracted with CH2Cl2 (3×25 mL). The combined organic extracts were washed with brine (25 mL), dried over Na2SO4, and concentrated. Flash chromatography (Biotage 25+M column, CH2Cl2/MeOH, 50:1 to 40:1) yielded 2-(3-(5-(2-oxo-4-(4-(trifluoromethyl)phenyl)pyridin-1(2H)-yl)-1H-indazol-1-yl)propyl)isoindoline-1,3-dione. 2-(3-(5-(2-oxo-4-(4-(trifluoromethyl)phenyl)pyridin-1(2H)-yl)-1H-indazol-1-yl)propyl)isoindoline-1,3-dione (73 mg, 0.13 mmol) was dissolved in ethanolamine (1.0 mL) and stirred at ambient temperature for 18 h. The reaction was concentrated. Flash column chromatography (Biotage 25+M column, CH2Cl2/MeOH/NH4OH, 30:1:0.1 to 10:1:0.2) yielded 1-(1-(3-aminopropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one. 1-(1-(3-aminopropyl)-1H-indazol-5-yl)-4-(4-(trifluoromethyl)phenyl)pyridin-2(1H)-one was dissolved in CH2Cl2 (1.0 mL) and Et3N (30 μL, 0.22 mmol), and di-tert-butyl dicarbonate (26 mg, 0.12 mmol) were added. The resulting solution was stirred at ambient temperature for 18 h. The reaction was concentrated. Flash column chromatography (silica gel, CH2Cl2/MeOH, 40:1) afforded tert-butyl-3-(5-(2-oxo-4-(4-(trifluoromethyl)phenyl)pyridin-1(2H)-yl)-1H-indazol-1-yl)propylcarbamate. Tert-butyl-3-(5-(2-oxo-4-(4-(trifluoromethyl)phenyl)pyridin-1(2H)-yl)-1H-indazol-1-yl)propylcarbamate was dissolved in CH2Cl2 (1.0 mL) and TFA (25 μL, 0.33 mmol). The resulting solution was stirred at ambient temperature for 18 h. The reaction was diluted with CH2Cl2 (10 mL) and washed with saturated NaHCO3. The organic solution was dried over Na2SO4, filtered and concentrated. Flash column chromatography (silica gel, CH2Cl2/MeOH/NH4OH, 30:1:0.1 to 20:1:0.1) yielded the title compound (16 mg, 29%): 1H NMR (500 MHz, CDCl3) δ 8.03 (s, 1H), 7.77-7.74 (m, 5H), 7.58-7.44 (m, 3H), 6.92 (d, J=1.5 Hz, 1H), 6.53 (dd, J=7.5, 2.0 Hz, 1H), 4.54 (t, J=7.0 Hz, 2H), 2.70 (t, J=7.0 Hz, 2H), 2.10-2.04 (m, 2H).

後処理

  1. extractionextracted with EtOAc (3×25 mL)
  2. washThe extracts were washed with brine (25 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-daca7593c44f45f38d042200eeca615f
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273770B2

反応ノート

読み込み中…

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