反応 #60441

ord-fcef352092914a9180b75372ac6574b1

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出The mixture was then extracted with ethyl acetate
  2. 2
    濃縮The separated organic layer was concentrated under reduced pressure

実験手順

(S)-4-[2-(4,4-Diethylcyclohexyl)-4-(3-methoxypiperidin-1-yl)phenyl]piperazine-1-carboxylic acid t-butyl ester (59 mg, 0.1148 mmol) produced in Example (50b) was dissolved in a mixed solvent of dichloromethane (0.7 mL)-water (1 drop). Trifluoroacetic acid (0.177 mL, 2.296 mmol) was added thereto followed by stirring for 15 hours and 20 minutes under the same conditions. Aqueous solution of potassium carbonate was added to the reaction mixture to make the mixture basic. The mixture was then extracted with ethyl acetate. The separated organic layer was concentrated under reduced pressure to give a crude product of (S)-1-[2-(4,4-diethylcyclohexyl)-4-(3-methoxypiperidin-1-yl)phenyl]piperazine as a brown oil. This was directly used without purification for the following reaction.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07425554B2uspto-grants-2008_09