反应详情

温度

0 °C

To a solution of (2-benzyloxy-4-chlorophenyl)-carbamic acid tert-butyl ester (14.75 g, 44.2 mmol) in DMF (150 mL) at 0° C. is added NaH (1.94 g, 60% in mineral oil, 48.6 mmol) and the mixture is stirred at 0° C. for 10 min. To this is added methyl bromoacetate (5.04 mL, 53 mmol) and the mixture is stirred at RT for 8 h. The mixture is poured into ice/water (150 mL) and is extracted with EtOAc (700 mL). The organic phase is washed with 1N HCl (3×150 mL) and brine (150 mL) then is dried over sodium sulfate. The solvent is removed under reduced pressure and the residue purified by flash chromatography using a gradient of 5-10% EtOAc/hexane as eluent to give the title compound.

1. stirringthe mixture is stirred at RT for 8 h
2. extractionis extracted with EtOAc (700 mL)
3. washThe organic phase is washed with 1N HCl (3×150 mL) and brine (150 mL)
4. dry with materialthen is dried over sodium sulfate
5. customThe solvent is removed under reduced pressure
6. customthe residue purified by flash chromatography