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Potassium Carbonate → 4,6-Difluoro-5-(4-(1-hydroxycyclobutyl)phenyl)-1H-indole-3-carbaldehyde

HRID 338231
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 338231
CC1(C)COB(B2OCC(C)(C)CO2)OC1.C([O-])(=O)C.[K+].Br[C:23]1[CH:28]=[CH:27][C:26]([C:29]2([OH:33])[CH2:32][CH2:31][CH2:30]2)=[CH:25][CH:24]=1.Br[C:35]1[C:36]([F:47])=[C:37]2[C:41](=[CH:42][C:43]=1[F:44])[NH:40][CH:39]=[C:38]2[CH:45]=[O:46].C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2].CCO.C1(C)C=CC=CC=1>[F:47][C:36]1[C:35]([C:23]2[CH:28]=[CH:27][C:26]([C:29]3([OH:33])[CH2:32][CH2:31][CH2:30]3)=[CH:25][CH:24]=2)=[C:43]([F:44])[CH:42]=[C:41]2[C:37]=1[C:38]([CH:45]=[O:46])=[CH:39][NH:40]2
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

10

Edukt 5

HCID 11430Potassium CarbonateHCID 517044Potassium AcetateHCID 2734316Bis(neopentyl glycolato)diboronHCID 120954191-(4-Bromophenyl)cyclobutanolHCID 866985785-Bromo-4,6-difluoro-1H-indole-3-carbaldehyde

Produkt 1

HCID 86698579
4,6-Difluoro-5-(4-(1-hydroxycyclobutyl)phenyl)-1H-indole-3-carbaldehyde
Ausbeute 66,5 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)Katalysator2×HCID 702EthanolLösungsmittelHCID 1140TolueneLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

A mixture of 5,5,5′,5′-tetramethyl-2,2′-bi(1,3,2-dioxaborinane) (188.0 mg, 0.55 mmol), oven dried potassium acetate (230.0 mg, 2.34 mmol), and 1-(4-bromophenyl)cyclobutanol (114.0 mg, 0.50 mmol) in 1,4-dioxane (2 mL) was degassed with N2 for 15 min, then treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (20.0 mg, 0.027 mmol). The reaction mixture was subjected to microwave irradiation at 110° C. for 1 hour. The cooled reaction mixture was filtered through celite, rinsed with EtOAc and concentrated to dryness. To the resulting dark solid ((45.0 mg, 0.17 mmol) was added 5-bromo-4,6-difluoro-1H-indole-3-carbaldehyde (45.0 mg, 0.17 mmol), 2N aqueous potassium carbonate (0.20 mL, 0.40 mmol), toluene (1.5 mL) and EtOH (0.5 mL). The reaction mixture was degassed with N2 for 10 minutes, treated with [1,1′-bis(diphenylphosphino)ferrocene]dichloropalladium(II) (14.0 mg, 0.019 mmol), and heated in a sealed pressure tube at 110° C. for 2 hours. The reaction mixture was cooled to room temperature and purified by flash chromatography (0-67% EtOAc/heptanes) to give the title compound (37 mg, 65%) as a white solid. MS (ES+) 328.0 (M+H)+. 1H NMR (500 MHz, CD3OD) δ 10.04 (d, J=2.68 Hz, 1H), 8.15 (s, 1H), 7.64 (d, J=8.05 Hz, 2H), 7.48 (d, J=8.05 Hz, 2H), 7.21 (d, J=9.51 Hz, 1H), 2.57-2.66 (m, 2H), 2.39-2.46 (m, 2H), 2.03-2.12 (m, 1H), 1.73-1.83 (m, 1H).

Aufarbeitung

  1. customwas degassed with N2 for 15 min
  2. customirradiation at 110° C. for 1 hour
  3. customThe cooled reaction mixture
  4. filtrationwas filtered through celite
  5. washrinsed with EtOAc
  6. concentrationconcentrated to dryness
  7. customThe reaction mixture was degassed with N2 for 10 minutes
  8. temperatureThe reaction mixture was cooled to room temperature
  9. custompurified by flash chromatography (0-67% EtOAc/heptanes)

Quellen und Nachweise

ORD-Eintrag
ord-f97e183b811843bc969b563d9a509c05
Quelldatensatz
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08889730B2

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