Reaktion #678562

ord-f177f0317dbd40f89e215311cff2a6cf

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeUnder a nitrogen atmosphere, into a reaction vessel equipped with a dropping funnel
  2. 2
    Sonstigea solution obtained
  3. 3
    workup.ADDITIONwas dropped at −78° C
  4. 4
    SonstigeThe resultant reaction mixture
  5. 5
    Einengenwas concentrated
  6. 6
    Sonstigepurified by silica gel column chromatography

Vorschrift

Under a nitrogen atmosphere, into a reaction vessel equipped with a dropping funnel were added 0.91 g of 2-bromoanisole and 20 mL of tetrahydrofuran. The resultant solution was cooled down to −78° C., then, 3.4 ml of n-butyllithium (1.62 M/hexane solution) was dropped. The resultant mixture was stirred at the same temperature for 2 hours, then, a solution obtained by dissolving 1.00 g of chlorodicyclopentylphosphine in 13 ml of tetrahydrofuran was dropped at −78° C. The resultant mixture was stirred at room temperature for 3 hours. The resultant reaction mixture was concentrated, and purified by silica gel column chromatography, to obtain 1.19 g of dicyclopentyl(2-methoxyphenyl)phosphine in the form of viscous liquid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09238665B2uspto-grants-2016_01