Reaktion #1437546

ord-9278b8cc5ea34029aa6890f4327ea54c

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationfilter the palladium on carbon
  2. 2
    Einengenconcentrate the filtrate
  3. 3
    SonstigePurify by silica gel chromatography

Vorschrift

Dissolve (S)-1,4-dibenzyl-2-(2-pyridinyl-ethyl)-piperazine (2.14 g, 5.76 mmol) in ethanol (40 mL). Add ammonium formate (2.18 g, 34.6 mmol) and palladium (430 mg, 5 wt. % on carbon) and heat to reflux. After 6 hours 30 minutes, filter the palladium on carbon and concentrate the filtrate. Purify by silica gel chromatography using 7N ammonia in methanol-methylene chloride (5%–15%) as the eluent to give 945 mg (86%) of the title compound: mp 113–116° C.; mass spectrum (ion spray): m/z=192 (M+1). Analysis calculated for C11H17N3: C, 69.07; H, 8.96; N, 21.97. Found: C, 69.08; H, 8.77; N, 21.81.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07214673B2uspto-grants-2007_05