Reaktion #480560

ord-896fcd5b235542c6852ef646485e65d7

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeQuenching with water
  2. 2
    Extraktionwas followed by extraction with ethyl acetate
  3. 3
    TrocknenThe combined organic extracts were dried with sodium sulfate
  4. 4
    Einengenconcentrated

Vorschrift

To a solution of 0.27 g (0.87 mmol) N-methyl-6-morpholin-4-yl-4-o-tolyl-nicotinamide in 15 ml tetrahydrofuran, 1.12 ml of a 1 M solution (1.12 mmol) of potassium hexamethyldisilazide in tetrahydrofuran was added at 0° C. After 30 min, 0.16 ml (0.87 mmol) 3,5-bis(trifluoromethyl)benzyl bromide were added dropwise and the reaction mixture was allowed to warm to room temperature over night. Quenching with water was followed by extraction with ethyl acetate. The combined organic extracts were dried with sodium sulfate and concentrated. Column chromatography gave 0.20 g (44%) of the title compound as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06806370B2uspto-grants-2004_10