Reaktion #46215

ord-f4b9ea477d1d4b3a99876108ba284927

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe organic layer was separated
  2. 2
    Extraktionthe aqueous phase was extracted with dichloromethane (50 mL×3)
  3. 3
    WaschenThe combined organic layers were washed with NaHCO3 (sat solution), water and brine
  4. 4
    Trocknendried over Na2SO4
  5. 5
    Einengenconcentrated to dryness

Vorschrift

A mixture of (2,3-dihydro-benzo[1,4]dioxin-6-yl)methanol (10.6 g) in SOCl2 (10 mL) was stirred at room temperature for 10 min and then poured into ice-water. The organic layer was separated and the aqueous phase was extracted with dichloromethane (50 mL×3). The combined organic layers were washed with NaHCO3 (sat solution), water and brine, dried over Na2SO4 and concentrated to dryness to obtain 6-chloromethyl-2,3-dihydro-benzo[1,4]dioxine (12 g, 88% over two steps), which was used directly in next step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741321B2uspto-grants-2010_06