반응 #629479

ord-fec00548e9594f54a1fa2b6c8f8a6f31

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture is then filtered
  2. 2
    농축the filtrate is concentrated under reduced pressure
  3. 3
    workup.DISTILLATIONthe crude product is distilled under reduced pressure

실험 절차

A solution of 17.0 g of ethyl 2-cyanopropyl(diethoxymethyl)phosphinate in 150 ml of ethanol is added to 155 g of an 8% solution of ammonia in ethanol. To this are added 10 ml of Raney Nickel and the resulting mixture is hydrogenated at 1 bar until the theoretical amount of hydrogen has been taken up. The mixture is then filtered, the filtrate is concentrated under reduced pressure and the crude product is distilled under reduced pressure to give ethyl 3-amino-2-methylpropyl(diethoxymethyl)phosphinate, b.p. 150° C./0.01 mbar, 31P=+45.8 and +45.7 ppm (CDCl3).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04656298uspto-grants-1987_04