Reaktion #1010551

ord-1d019067ccbd417db4610b2cbf2487a0

Lösungsmittel

Reaktionsbedingungen

Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeevaporated
  2. 2
    Sonstigepurified by chromatography (silica gel, gradient 0-30% dichloromethane in hexane)

Vorschrift

N,N-diisopropylethylamine (184 mL) was added to a solution of 2-nitro-1-(2,5-difluorophenyl)ethanone (92.7 g, 461 mmol) in N,N-dimethylformamide (1000 mL) and 3-iodo-2-(iodomethyl)prop-1-ene (156 g, 507 mmol). The mixture was heated at 60° C. for 2 h, evaporated and purified by chromatography (silica gel, gradient 0-30% dichloromethane in hexane) to yield 3-methylene-5-nitro-6-(2,5-difluorophenyl)-3,4-dihydro-2H-pyran.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09278976B2uspto-grants-2016_03