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Cesium carbonate → ethyl 3-(2-(4-fluoro-1H-indol-2-yl)-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)pyridin-3-yl)propanoate

HRID 595744
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HRID 595744 반응식
Cl[C:2]1[C:7]([CH2:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:6][CH:5]=[C:4]([C:15]2[C:16]([N:35]([CH3:40])[S:36]([CH3:39])(=[O:38])=[O:37])=[CH:17][C:18]3[O:22][C:21]([C:23]4[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=4)=[C:20]([C:30](=[O:33])[NH:31][CH3:32])[C:19]=3[CH:34]=2)[N:3]=1.[F:41][C:42]1[CH:50]=[CH:49][CH:48]=[C:47]2[C:43]=1[CH:44]=[C:45](B1OC(C)(C)C(C)(C)O1)[NH:46]2.C(=O)([O-])[O-].[Cs+].[Cs+].O1CCOCC1>CC(P(C(C)(C)C)[C]1[CH][CH][CH][CH]1)(C)C.CC(P(C(C)(C)C)[C]1[CH][CH][CH][CH]1)(C)C.Cl[Pd]Cl.[Fe].O>[F:41][C:42]1[CH:50]=[CH:49][CH:48]=[C:47]2[C:43]=1[CH:44]=[C:45]([C:2]1[C:7]([CH2:8][CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:6][CH:5]=[C:4]([C:15]3[C:16]([N:35]([CH3:40])[S:36]([CH3:39])(=[O:38])=[O:37])=[CH:17][C:18]4[O:22][C:21]([C:23]5[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=5)=[C:20]([C:30](=[O:33])[NH:31][CH3:32])[C:19]=4[CH:34]=3)[N:3]=1)[NH:46]2
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참가 물질

7

반응물 4

HCID 10796Cesium carbonateHCID 312751,4-DioxaneHCID 532172124-Fluoro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-YL)-1H-indoleHCID 90332427ethyl 3-(2-chloro-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)pyridin-3-yl)propanoate

생성물 1

HCID 90333603
ethyl 3-(2-(4-fluoro-1H-indol-2-yl)-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)pyridin-3-yl)propanoate

시약·촉매·용매 2

HCID 178454869HCID 178454869, 화합물촉매HCID 962Water용매

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온도
90 °C

실험 절차

To a mixture of ethyl 3-(2-chloro-6-(2-(4-fluorophenyl)-3-(methylcarbamoyl)-6-(N-methylmethylsulfonamido)benzofuran-5-yl)pyridin-3-yl)propanoate (120 mg, 0.204 mmol), 4-fluoro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-indole (80 mg, 0.306 mmol), cesium carbonate (133 mg, 0.408 mmol) and dichloro[1,1′-bis(di-t-butylphosphino)ferrocene]palladium (II) (13.3 mg, 0.02 mmol) was added 1,4-dioxane (1.86 mL) and H2O (0.186 mL). A steady stream of N2 was bubbled through the reaction mixture for 5 minutes then the mixture was heated to 90° C. for 9 h. The mixture was cooled to ambient temperature, diluted with EtOAc, and washed successively with H2O (1×) and brine (1×). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography using a gradient of 0-100% EtOAc/Hexanes as eluent and further purified by silica gel column chromatography using a step gradient of 0-20-80% EtOAc/CH2Cl2 as eluent. MS (M+H)+: 687.

후처리

  1. customA steady stream of N2 was bubbled through the reaction mixture for 5 minutes
  2. temperatureThe mixture was cooled to ambient temperature
  3. additiondiluted with EtOAc
  4. washwashed successively with H2O (1×) and brine (1×)
  5. dry with materialThe organic layer was dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by silica gel column chromatography
  9. customfurther purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-4a2347ca916e444fa038153b33d1e80c
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09243002B2

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