Reaktion #218644

ord-6e0ccf2b342e4947a5c95f5b1361b281

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationFilter
  2. 2
    Sonstigeevaporate the solvent

Vorschrift

Stir (R)-10-(3-allyloxymethyl-4-methyl-piperazin-1-yl)-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene (270 mg), 20% palladium hydroxide (Degaussa type, 15 mg) in ethanol (0.014M)) under hydrogen atmosphere (1 atm) for 4 hours at room temperature. Filter and evaporate the solvent to afford the title compound as a yellow solid (268 mg): 1H NMR (CDCl3) δ 0.90 (t, 3H), 1.58 (m, 2H), 2.30 (s, 3H), 2.33 (m, 2H), 2.39 (s, 3H), 2.84 (m, 2H), 3.14 (t, 1H), 3.38 (t, 2H), 3.49 (d, 1H), 3.58 (d, 1H), 3.95 (d, 1H), 4.07 (d, 1H), 4.94 (s, 1H), 6.31 (s, 1H), 6.60 (d, 1H), 6.85 (t, 1H), 6.95 (t, 1H), 7.02 (d, 1H); MS (ESI) m/z (rel intensity) 385 (100).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07384934B2uspto-grants-2008_06