Reaktion #160076

ord-ba41d3bd349f49a4bd57eab1f18b7534

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was decanted
  2. 2
    Sonstigethe residue was triturated with methanol and hexanes
  3. 3
    EinengenThe solvent was concentrated in vacuo

Vorschrift

To a solution of tert-butyl 8-ethyl-9-phenyl-11-oxa-3,8-diazaspiro[5.5]undecane-3-carboxylate (295 mg, 0.82 mmol) in DCM (3 mL) was added hydrogen chloride (2 mL of 4 M dioxane, 8.18 mmol). The reaction mixture was stirred for 1 hour. The solvent was decanted and the residue was triturated with methanol and hexanes. The solvent was concentrated in vacuo to obtain 8-ethyl-9-phenyl-11-oxa-3,8-diazaspiro[5.5]undecane hydrochloride salt (230 mg, 95%) as a fluffy solid. ESI-MS m/z calc. 260.2. Found 261.1 (M+1)+; Retention time: 0.2 minutes (3 min run).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08828996B2uspto-grants-2014_09