反应详情

1,1-dimethylethyl [2-({[4-(bromomethyl)phenyl]carbonyl}amino)-4-(2-thienyl)phenyl]carbamate (500 mg, 1.026 mmol), diethyl (aminomethyl)phosphonate oxalate (791 mg, 3.08 mmol), and DIPEA (1.254 mL, 7.18 mmol) were stirred in DMF (6 mL) at 50° C. overnight. Room temperature was attained, H2O: was added and the products extracted into EtOAc (×2). The combined organic extracts were washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by MPLC (0-10% MeOH-EtOAc) gave diethyl [({[4-({[2-({[(1,1-dimethylethyl)oxy]carbonyl}amino)-5-(2-thienyl)phenyl]amino}carbonyl)phenyl]methyl}amino)methyl)phosphonate as a colourless gum. MS: cal'd 574 (MH+), exp 574.

1. customRoom temperature
2. extractionthe products extracted into EtOAc (×2)
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customPurification of the residue by MPLC (0-10% MeOH-EtOAc)