Reaktion #40528

ord-56dffb8badf046c4b6812a170c7583af

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGthe reaction stirred at room temperature 3 days
  2. 2
    EinengenThe pale yellow solution was concentrated
  3. 3
    Sonstigeto afford an oily residue, which
  4. 4
    Sonstigewas triturated with ether
  5. 5
    FiltrationThe solids were collected by suction filtration
  6. 6
    Sonstigedried in vacuo

Vorschrift

The 3,3-dimethyl-4-oxo-piperidine-1-carboxylic acid tert-butyl ester thus prepared (450 mg, 1.97 mmol) was dissolved in methylene chloride (10 mL). Trifluoroacetic acid was added (305 uL) and the resulting solution stirred at room temperature 2 h. Additional trifluoroacetic acid was added (300 uL) and the reaction stirred at room temperature 3 days. The pale yellow solution was concentrated to afford an oily residue, which was triturated with ether. The solids were collected by suction filtration and dried in vacuo. 3,3-Dimethyl-piperidin-4-one was isolated and used as its trifluoroacetic acid salt (381 mg, 80%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07727985B2uspto-grants-2010_06