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Cesium carbonate → HCID 86684750, Verbindung

HRID 2401159
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2401159
Br[C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:13]=[C:12]3[N:14]=[C:15]([O:17][CH:18]4[CH:22]5[O:23][CH2:24][CH:25]([OH:26])[CH:21]5[O:20][CH2:19]4)[NH:16][C:11]3=[CH:10][C:9]=2[Cl:27])=[CH:4][CH:3]=1.[C:28]([CH:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)#[CH:29].C(=O)([O-])[O-].[Cs+].[Cs+]>[Cu]I>[Cl:27][C:9]1[CH:10]=[C:11]2[NH:16][C:15]([O:17][C@H:18]3[C@H:22]4[O:23][CH2:24][C@@H:25]([OH:26])[C@H:21]4[O:20][CH2:19]3)=[N:14][C:12]2=[N:13][C:8]=1[C:5]1[CH:6]=[CH:7][C:2]([C:29]#[C:28][CH:30]2[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]2)=[CH:3][CH:4]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 10796Cesium carbonateHCID 52462504-ethynylpiperidineHCID 77462307HCID 77462307, Verbindung

Produkt 1

HCID 86684750HCID 86684750, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)Katalysator

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

3R,3aR,6R,6aR)-6-((5-(4-bromophenyl)-6-chloro-1H-imidazo[4,5-b]pyridin-2-yl)oxy)hexahydrofuro[3,2-b]furan-3-ol (25 mg, 0.055 mmol), 4-ethynylpiperidine (10.5 mg, 0.072 mmol), copper (I) iodide (2.1 mg, 0.011 mmol), chloro(tri-tert-butyl)-2-[-(2′amino-1,1′-biphenyl)]palladium (II) (5.7 mg, 0.011 mmol, prepared by a procedure analogous to procedures described in J. AM. CHEM. SOC. 2010, 132, 14073-14075), and cesium carbonate (54.0 mg, 0.166 mmol) were placed under nitrogen in dry, degassed toluene (138 μl) and dimethylacetamide (138 μl). The mixture was stirred at 50° C. for 2 hours. The resulting residue was diluted with dimethylformamide (0.7 mL), then filtered through a filter disc (0.45 micron). The material was purified by reverse phase HPLC purification using 0-100% acetonitrile in water over 10 minutes. The desired product fraction was concentrated under reduced pressure to afford the title compound as an off-white solid. LC-MS: calculated for C25H25ClN4O4 480.16 observed m/e: 481.14 (M+H)+ (Rt 1.43/4 min). 1H NMR δ (ppm) (CD3OD): 7.80 (1H, s), 7.62 (2H, d, J=8.5 Hz), 7.49 (2H, d, J=8.5 Hz), 5.53 (1H, m), 4.95 (1H, t, J=5.5 Hz), 4.46 (1H, t, J=5.0 Hz), 4.27 (1H, m), 4.15 (1H, dd, J=9.5, 6.0 Hz), 4.09 (1H, dd, J=10.0, 4.9 Hz), 3.88 (1H, dd, J=8.0, 7.0 Hz), 3.58 (1H, t, J=8.5 Hz), 3.42 (2H, m), 3.18 (2H, m), 3.09 (1H, m), 2.17 (2H, m), 1.96 (2H, m)

Aufarbeitung

  1. customin dry
  2. customdegassed toluene (138 μl) and dimethylacetamide (138 μl)
  3. additionThe resulting residue was diluted with dimethylformamide (0.7 mL)
  4. filtrationfiltered through a filter disc (0.45 micron)
  5. customThe material was purified by reverse phase HPLC purification
  6. customover 10 minutes
  7. concentrationThe desired product fraction was concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-314259c3c65e4e61a5b7a14c46f5951c
Quelldatensatz
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08796258B2

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