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Acetonitrile → 3-(2-Bromophenyl)propanenitrile

HRID 716946
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 716946
[C:1](#[N:3])[CH3:2].[Li]CCCC.[Br:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16]Br>O1CCCC1>[Br:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][CH2:2][C:1]#[N:3]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6342AcetonitrileHCID 769652-Bromobenzyl bromideHCID 178418339Butyllithium

Produkt 1

HCID 133082983-(2-Bromophenyl)propanenitrile

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel2×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

Into a 500-mL 3-necked round-bottom flask, was placed a solution of acetonitrile (49 g, 1.20 mol, 9.96 equiv) in tetrahydrofuran (150 mL). This was followed by the addition of BuLi (72 mL, 1.50 equiv) dropwise with stirring at −78° C. Stirred at −78° C. for 1 h. To this was added a solution of 1-bromo-2-(bromomethyl)benzene (30 g, 120.00 mmol, 1.00 equiv) in tetrahydrofuran (100 mL) dropwise with stiffing at −78° C. The resulting solution was stirred for 1 h at −78° C. The reaction was quenched by the addition of 100 mL of water at −78° C. The resulting aqueous solution was extracted with 3×100 mL of ethyl acetate and the organic layers combined and dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:20). The crude product was purified by distillation under reduced pressure (2 mm Hg) and the fraction was collected at 98-107° C. This resulted in 13.21 g (52%) of 3-(2-bromophenyl)propanenitrile as colorless oil.

Aufarbeitung

  1. customInto a 500-mL 3-necked round-bottom flask, was placed
  2. stirringStirred at −78° C. for 1 h
  3. customwith stiffing at −78° C
  4. stirringThe resulting solution was stirred for 1 h at −78° C
  5. customThe reaction was quenched by the addition of 100 mL of water at −78° C
  6. extractionThe resulting aqueous solution was extracted with 3×100 mL of ethyl acetate
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under vacuum
  9. distillationThe crude product was purified by distillation under reduced pressure (2 mm Hg)
  10. customthe fraction was collected at 98-107° C
  11. customThis resulted in 13.21 g (52%) of 3-(2-bromophenyl)propanenitrile as colorless oil

Quellen und Nachweise

ORD-Eintrag
ord-ea1afd01c4c84facbc433eac4a4d9c17
Quelldatensatz
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09193693B2

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