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Diisopropylethylamine → (R)-1-(1-(5-cyanopyridin-3-yl)propyl)-1H-indole-4,5-dicarbonitrile

HRID 1851141
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1851141
Cl.[NH2:2][C@@H:3]([C:6]1[CH:7]=[N:8][CH:9]=[C:10]([CH:13]=1)[C:11]#[N:12])[CH2:4][CH3:5].CCN(C(C)C)C(C)C.[C:23]([C:25]1[C:32](F)=[CH:31][CH:30]=[C:27]([C:28]#[N:29])[C:26]=1[C:34]#[N:35])#[CH:24].C([O-])(O)=O.[Na+]>CCOC(C)=O.[Cu]I.CN1C(=O)CCC1>[C:11]([C:10]1[CH:13]=[C:6]([C@H:3]([N:2]2[C:32]3[C:25](=[C:26]([C:34]#[N:35])[C:27]([C:28]#[N:29])=[CH:30][CH:31]=3)[CH:23]=[CH:24]2)[CH2:4][CH3:5])[CH:7]=[N:8][CH:9]=1)#[N:12]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 867091973-Ethynyl-4-fluorophthalonitrileHCID 86709199(R)-5-(1-aminopropyl)nicotinonitrile hydrochloride

Produkt 1

HCID 86709198(R)-1-(1-(5-cyanopyridin-3-yl)propyl)-1H-indole-4,5-dicarbonitrileAusbeute 35,1 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)KatalysatorHCID 8857Ethyl AcetateLösungsmittelHCID 13387N-methyl-2-pyrrolidoneLösungsmittel

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

To a solution of (R)-5-(1-aminopropyl)nicotinonitrile hydrochloride (0.081 g, 0.411 mmol) in anhyd NMP (2.0 mL) was added DIEA (0.215 mL, 1.232 mmol) via syringe. The mixture was stirred 15 min and 3-ethynyl-4-fluorophthalonitrile (0.0635 g, 0.373 mmol) was added in one portion. The mixture was stirred at rt under N2 for 36 h, poured into satd NaHCO3 and extracted with EtOAc (×3). Combined organics were washed (water, brine), dried over Na2SO4 and concentrated in vacuo. The residue was dissolved in anhyd DMF (3 mL), CuI (0.036 g, 0.187 mmol) was added and the mixture was subjected to microwave heating (140° C.) for 30 min. The mixture was diluted with EtOAc and filtered through a pad of Celite. The filtrate was diluted 1:1 with heptane and concentrated in vacuo (3× heptane chase). The residue was purified by low pressure liquid chromatography (silica gel, EtOAc/hexanes, gradient elution) affording (R)-1-(1-(5-cyanopyridin-3-yl)propyl)-1H-indole-4,5-dicarbonitrile (0.0407 g, 0.131 mmol, 35.0% yield) as a yellow gum: 1H NMR (400 MHz, CDCl3) δ 8.83 (d, J=8.7 Hz, 1H), 8.69 (d, J=2.2 Hz, 1H), 7.66 (t, J=2.1 Hz, 1H), 7.63 (d, J=3.4 Hz, 1H), 7.53 (s, 2H), 7.00 (d, J=3.4 Hz, 1H), 5.50 (dd, J=8.7, 6.8 Hz, 1H), 2.53-2.34 (m, 2H), 1.03 (t, J=7.3 Hz, 3H); MS (LCMS ES+) m/z 312 ([M+H]+, 6%), 353 ({[M+H]+MeCN}+, 100%).

Aufarbeitung

  1. stirringThe mixture was stirred at rt under N2 for 36 h
  2. extractionextracted with EtOAc (×3)
  3. washCombined organics were washed (water, brine)
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. dissolutionThe residue was dissolved in anhyd DMF (3 mL)
  7. filtrationfiltered through a pad of Celite
  8. additionThe filtrate was diluted 1:1 with heptane
  9. concentrationconcentrated in vacuo (3× heptane chase)
  10. customThe residue was purified by low pressure liquid chromatography (silica gel, EtOAc/hexanes, gradient elution)

Quellen und Nachweise

ORD-Eintrag
ord-1576438d52a54bbb877975640384d03c
Quelldatensatz
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08957104B2

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