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Water → 5-Ethyl-7-methyl-4-(((tetrahydro-2H-pyran-2-yl)oxy)methyl)-1-tosyl-1H-indole

HRID 2173971
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HRID 2173971 반응식
Cl[C:2]1[C:3]([CH2:22][O:23][CH:24]2[CH2:29][CH2:28][CH2:27][CH2:26][O:25]2)=[C:4]2[C:8](=[C:9]([CH3:11])[CH:10]=1)[N:7]([S:12]([C:15]1[CH:21]=[CH:20][C:18]([CH3:19])=[CH:17][CH:16]=1)(=[O:14])=[O:13])[CH:6]=[CH:5]2.C(=O)([O-])[O-].[Cs+].[Cs+].[K].O.O1CCO[CH2:40][CH2:39]1>C(Cl)Cl>[CH2:39]([C:2]1[C:3]([CH2:22][O:23][CH:24]2[CH2:29][CH2:28][CH2:27][CH2:26][O:25]2)=[C:4]2[C:8](=[C:9]([CH3:11])[CH:10]=1)[N:7]([S:12]([C:15]1[CH:21]=[CH:20][C:18]([CH3:19])=[CH:17][CH:16]=1)(=[O:14])=[O:13])[CH:6]=[CH:5]2)[CH3:40]
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HCID 962WaterHCID 10796Cesium carbonateHCID 312751,4-DioxaneHCID 5462222PotassiumHCID 867015385-chloro-7-methyl-4-(((tetrahydro-2H-pyran-2-yl)oxy)methyl)-1-tosyl-1H-indole

생성물 1

HCID 867015405-Ethyl-7-methyl-4-(((tetrahydro-2H-pyran-2-yl)oxy)methyl)-1-tosyl-1H-indole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
90 °C

실험 절차

To a suspension of (±)-5-chloro-7-methyl-4-(((tetrahydro-2H-pyran-2-yl)oxy)methyl)-1-tosyl-1H-indole (Example 47-D) (200 mg, 0.46 mmol), cesium carbonate (601 mg, 1.8 mmol), potassium ethylrifluoroborate (125 mg, 0.92 mmol) in dioxane (3 mL)/H2O (0.3 mL) Pd(OAc)2 (21 mg, 0.092 mmol) and Ru-Phos (CAS 787618-22-8, 86 mg, 0.18 mmol) were added and then the mixture was stirred at 90° C. for 15 h. The reaction mixture was cooled to room temperature, and diluted with CH2Cl2. The organic phase was separated and washed with H2O, and brine, dried over Na2SO4, and then filtered. Concentration of the filtrate gave a residue that was purified by SiO2 column chromatography (heptane/EtOAc=1/0 to 3/2) to give the title compound. 1H NMR (400 MHz, ACETONITRILE-d3) δ 7.75 (d, J=3.79 Hz, 1H), 7.57 (d, J=8.34 Hz, 2H), 7.31 (d, J=8.34 Hz, 2H), 6.95 (s, 1H), 6.91 (d, J=3.79 Hz, 1H), 4.90 (d, J=11.24 Hz, 1H), 4.65 (d, J=11.24 Hz, 1H), 4.61-4.64 (m, 1H), 3.79-3.92 (m, 1H), 3.41-3.54 (m, 1H), 2.71 (q, J=7.58 Hz, 2H), 2.53 (s, 3H), 2.35 (s, 3H), 1.56-1.75 (m, 2H), 1.38-1.56 (m, 4H), 1.16 (t, J=7.58 Hz, 3H).

후처리

  1. additionwere added
  2. temperatureThe reaction mixture was cooled to room temperature
  3. customThe organic phase was separated
  4. washwashed with H2O, and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customConcentration of the filtrate gave a residue that
  8. customwas purified by SiO2 column chromatography (heptane/EtOAc=1/0 to 3/2)

출처 및 근거

ORD 기록
ord-9a0206a382bf4da98da0f1942029e249
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056874B2

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