Reaktion #11524

ord-760b60ae9f0d4a8cb3a157644a6f1fab

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe solid was filtered off
  2. 2
    Waschenwashed with THF
  3. 3
    Sonstigethe filtrate evaporated
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in ethyl acetate
  5. 5
    Waschenwashed with 1N hydrochloric acid, water, brine
  6. 6
    Trocknendried (MgSO4)
  7. 7
    WaschenChromatography on flash silica, eluting with 0 to 25% ethyl acetate in isohexane

Vorschrift

3-Bromophenylethylamine hydrochloride (9.44 g) was added to THF (60 ml) containing triethylamine (12.24 ml) and stirred-under argon at 5° C. during the portionwise addition over 15 minutes of 4-methylphenylsulphonyl chloride (11.44 g). The slurry was diluted with THF (50 ml) and stirred for 16 h. The solid was filtered off, washed with THF and the filtrate evaporated. The residue was dissolved in ethyl acetate, washed with 1N hydrochloric acid, water, brine and dried (MgSO4). Chromatography on flash silica, eluting with 0 to 25% ethyl acetate in isohexane gave the product (9.67 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098240B2uspto-grants-2006_08