反応 #73926

ord-e8c798ffae5d46db97dd74bf33d753ae

反応条件

温度
50°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他A 250-mL pressure tank reactor was purged
  2. 2
    その他flushed
  3. 3
    温度maintained with a hydrogen atmosphere
  4. 4
    ろ過The solids were filtered out
  5. 5
    濃縮the resulting mixture was concentrated under vacuum

実験手順

A 250-mL pressure tank reactor was purged, flushed and maintained with a hydrogen atmosphere, then, was added a solution of ethyl 2-(benzyl((diethoxyphosphoryl)methyl)amino)acetate (8.0 g, 23.32 mmol, 1.00 equiv) in ethanol (180 mL), acetic acid (10 mL), Pd/C (0.9 g). The resulting solution was stirred at 20 atm for 32 h at 50° C. The solids were filtered out, and the resulting mixture was concentrated under vacuum. This resulted in 6.0 g (82%) of the acetic acid salt of ethyl 2-((diethoxyphosphoryl)methylamino)acetate as a brown oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541448B2uspto-grants-2013_09