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1-Bromo-2-methylpropane → 4-Methyl-2-(6-methylpyridin-3-yl)-pentanenitrile

HRID 512146
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Reaktionsgleichung

Reaktionsgleichung von HRID 512146
[H-].[Na+].[CH3:3][C:4]1[N:9]=[CH:8][C:7]([CH2:10][C:11]#[N:12])=[CH:6][CH:5]=1.Br[CH2:14][CH:15]([CH3:17])[CH3:16]>C1COCC1>[CH3:14][CH:15]([CH3:17])[CH2:16][CH:10]([C:7]1[CH:8]=[N:9][C:4]([CH3:3])=[CH:5][CH:6]=1)[C:11]#[N:12]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 65551-Bromo-2-methylpropaneHCID 24758Sodium hydrideHCID 114577152-(6-Methylpyridin-3-yl)acetonitrile

Produkt 1

HCID 867161684-Methyl-2-(6-methylpyridin-3-yl)-pentanenitrileAusbeute 64,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Versuchsvorschrift

To a cooled (0° C.) slurry of NaH (60% dispersion in oil, 2.74 g, 68.5 mmol) in THF (120 mL) was added a solution of (6-methylpyridin-3-yl)-acetonitrile (8.23 g, 62.3 mmol) in THF (60 mL). The mixture was stirred at room temperature for 3 h and then warmed to 40° C. for 1 h. The resulting reddish brown slurry was cooled to −20° C. and a solution of 1-bromo-2-methylpropane (8.53 g, 62.3 mmol) in THF (30 mL) was added dropwise and then stirred for 18 h at room temperature. The reaction was quenched with water and extracted with AcOEt. The organic extracts were combined and washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (15% EtOAc in hexane) to give 7.52 g (64% yield) of 4-methyl-2-(6-methylpyridin-3-yl)-pentanenitrile as an oil. 1H NMR (400 MHz, CDCl3) δ ppm 1.00 (dd, J=6.64, 4.30 Hz, 6 H), 1.53-1.70 (m, 1 El), 1.71-1.99 (m, 2 H), 2.57 (s, 3 H), 3.81 (dd, J=9.57, 6.45 Hz, 1 H), 7.19 (d, J=7.82 Hz, 1 H), 7.59 (dd, J=7.82, 2.34 Hz, 1 H), 8.43 (d, J=2.34 Hz, 1 H).

Aufarbeitung

  1. temperaturewarmed to 40° C. for 1 h
  2. temperatureThe resulting reddish brown slurry was cooled to −20° C.
  3. stirringstirred for 18 h at room temperature
  4. customThe reaction was quenched with water
  5. extractionextracted with AcOEt
  6. washwashed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by column chromatography on silica gel (15% EtOAc in hexane)

Quellen und Nachweise

ORD-Eintrag
ord-0a73d68e34a94fc3afba6ff84af6d637
Quelldatensatz
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09102591B2

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