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2-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenyl → N-(2,5-di-4-morpholinylphenyl)-5-fluoro-3,8-dimethyl-2-(2-pyridinyl)-4-quinolinamine

HRID 1431323
ノート
印刷プレビュー

反応式

HRID 1431323 の反応式
C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.O1CCN(C2C(N)=CC(N3CCOCC3)=CN=2)CC1.[O:54]1[CH2:59][CH2:58][N:57]([C:60]2[CH:66]=[CH:65][C:64]([N:67]3[CH2:72][CH2:71][O:70][CH2:69][CH2:68]3)=[CH:63][C:61]=2[NH2:62])[CH2:56][CH2:55]1.Cl[C:74]1[C:83]2[C:78](=[C:79]([CH3:85])[CH:80]=[CH:81][C:82]=2[F:84])[N:77]=[C:76]([C:86]2[CH:91]=[CH:90][CH:89]=[CH:88][N:87]=2)[C:75]=1[CH3:92].CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[N:57]1([C:60]2[CH:66]=[CH:65][C:64]([N:67]3[CH2:68][CH2:69][O:70][CH2:71][CH2:72]3)=[CH:63][C:61]=2[NH:62][C:74]2[C:83]3[C:78](=[C:79]([CH3:85])[CH:80]=[CH:81][C:82]=3[F:84])[N:77]=[C:76]([C:86]3[CH:91]=[CH:90][CH:89]=[CH:88][N:87]=3)[C:75]=2[CH3:92])[CH2:58][CH2:59][O:54][CH2:55][CH2:56]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 111557942-Dicyclohexylphosphino-2',4',6'-triisoprophylbiphenylHCID 23676156Sodium t-butoxideHCID 288098152,5-DimorpholinobenzenamineHCID 596310462,5-Dimorpholinopyridin-3-amineHCID 596312654-Chloro-5-fluoro-3,8-dimethyl-2-(pyridin-2-yl)quinoline

生成物 1

HCID 59631156
N-(2,5-di-4-morpholinylphenyl)-5-fluoro-3,8-dimethyl-2-(2-pyridinyl)-4-quinolinamine

試薬・触媒・溶媒 3

HCID 9811564Bis(dibenzylideneacetone)palladium触媒HCID 962Water溶媒HCID 1140Toluene溶媒

反応条件

温度
120 °C

実験手順

To a stirred solution of dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine (27.0 mg, 0.056 mmol), 2,5-dimorpholinopyridin-3-amine (37.0 mg, 0.140 mmol), 2,5-dimorpholinoaniline (55.0 mg, 0.21 mmol), 4-chloro-5-fluoro-3,8-dimethyl-2-(pyridin-2-yl)quinoline (100.0 mg, 0.35 mmol) and Pd2dba3 (13.0 mg, 0.014 mmol) in toluene (3.5 mL) was added sodium t-butoxide (84.0 mg, 0.87 mmol). The reaction mixture was heated to 120° C. and stirred for 45 min. The reaction was cooled to rt and diluted with water (25 mL). The mixture was extracted with EtOAc (3×10 mL) and DCM (1×10 mL). The organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo. The crude product was purified by column chromatography on silica gel (0 to 100% EtOAc in DCM) to give the desired products N-(2,5-di-4-morpholinylphenyl)-5-fluoro-3,8-dimethyl-2-(2-pyridinyl)-4-quinolinamine. 1H NMR (400 MHz, CDCl3) δ ppm 8.69 (1H, br. m.), 8.22 (1H br m), 8.02-8.12 (1H, m), 7.89 (1H, br. m.), 7.40 (2H, m), 7.28 (1H, m), 6.98-7.15 (2H, m), 6.24 (1H, br. s.), 3.87-4.00 (4H, br m), 3.80 (4H, br m), 3.09 (8H, br. m.), 2.77 (3H, s), 2.32 (3H, s); Mass Spectrum (ESI) m/e=514.3 (M+1). Further elution gave N-(2,5-di-4-morpholinyl-3-pyridinyl)-5-fluoro-3,8-dimethyl-2-(2-pyridinyl)-4-quinolinamine. 1H NMR (400 MHz, CDCl3) δ ppm 8.68 (1H, ddd, J=4.9, 1.8, 1.0 Hz), 8.08 (1H, d, J=7.8 Hz), 7.90 (1H, m), 7.82 (1H, br d), 7.60 (1H, d, J=2.5 Hz), 7.40-7.48 (1H, m), 7.37 (1H, m), 7.07 (1H, dd, J=13.6, 7.9 Hz), 6.47 (1H, br. s.), 3.88-4.00 (4H, m), 3.75-3.85 (4H, m), 3.23 (4H, br. s.), 3.03-3.13 (4H, m), 2.78 (3H, s), 2.31 (3H, s); Mass Spectrum (ESI) m/e=515.2 (M+1).

後処理

  1. temperatureThe reaction was cooled to rt
  2. extractionThe mixture was extracted with EtOAc (3×10 mL) and DCM (1×10 mL)
  3. dry with materialThe organic layers were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe crude product was purified by column chromatography on silica gel (0 to 100% EtOAc in DCM)

出典と根拠

ORDレコード
ord-30a9aee1ee764b309bb2c15bffee59ec
出典データセット
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08940724B2

反応ノート

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