反応 #83191

ord-fdccd8bfd6fb40e0ae64c2c4500e6029

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 4 hours
  2. 2
    濃縮The reaction mixture was concentrated under reduced pressure
  3. 3
    workup.DISSOLUTIONThe residue was dissolved in water (5.0 ml)

実験手順

A solution of tetraethyl (E,E)-farnesylaminomethylenebisphosphonate (2.42 g) in ethanol (25 ml) was added to a solution of sodium hydroxide (0.40 g) in ethanol (25 ml). The mixture was stirred under reflux for 4 hours. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in water (5.0 ml). The solution was subjected to ion-exchange chromatography [Amberlite CG-50 (H+ -type)] to obtain (E,E)-farnesylaminomethylenebisphosphonic acid diethyl ester disodium salt (0.75 g, 29%). Colorless powder, mp: 116°-118° C. Elemental Analysis for C20H37NO6P2Na2.5/2H2O: Calcd.: C, 44.45; H, 7.83; N, 2.59 Found: C, 44.08; H, 7.60; N, 2.59

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05624917uspto-grants-1997_04