反応 #5279

ord-a5f9fd3310074c17a1faf12c0f5dc92c

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The mixture is then filtered
  2. 2
    濃縮the filtrate is concentrated under reduced pressure
  3. 3
    その他The crude product is chromatographed on silica gel

実験手順

A solution of 3.45 g of ethyl 3-amino-2-phenylpropyl(diethoxymethyl)phosphinate in 25 ml of tertiary butanol is added to 2.0 g of 5% rhodium in alumina, suspended in 25 ml of tertiary butanol. The resulting mixture is hydrogenated at an atmosphere of 150 bar and temperature of 100° C. for a period of 20 hours. The mixture is then filtered and the filtrate is concentrated under reduced pressure. The crude product is chromatographed on silica gel using ethanol as eluent to give ethyl 3-amino-2-cyclohexylpropyl(diethoxymethyl)phosphinate as a viscous oil, 31P=47.1 and +47.0 ppm (CDCl3).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05243062uspto-grants-1993_09