Reaktion #10249

ord-30dde6a9126b43dba9aa60452e83156e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionextracted with chloroform
  2. 2
    Waschenwashed with distilled water
  3. 3
    Trocknenan aqueous saturated sodium bicarbonate solution and saturated saline and dried with anhydrous sodium sulfate
  4. 4
    SonstigeThe product was purified with silica gel column chromatography (chloroform)

Vorschrift

A solution of 0.3 g (0.91 mmol) of the obtained 2-chloro-1,2,3,4-tetrahydro-3-phenylsulfonyl-1,4-ethanonaphthalene and 15 ml of anhydrous THF was cooled to 0° C., added with 2.5 ml of 1,8-diazabicyclo[5.4.0]-7-undecene and stirred for 30 minutes. The solution is then added with a dilute hydrochloric acid solution, extracted with chloroform, washed with distilled water, an aqueous saturated sodium bicarbonate solution and saturated saline and dried with anhydrous sodium sulfate. The product was purified with silica gel column chromatography (chloroform) to obtain 1,4-dihydro-2-phenylsulfony-1,4-ethanonaphthalene (0.264 g, 0.89 mmol, yield: 98%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094625B2uspto-grants-2006_08