反应详情

温度

0 °C

1.0 g (3.2 mmol) of the compound from Example I are dissolved in 15 ml of DMF and treated under argon with 180 mg of NaH. The mixture is stirred at 0° C. for 15 minutes. 0.51 ml (6.2 mmol) of MeI is then added dropwise and the mixture is stirred again for 30 min. It is treated successively with H2O and ethyl acetate and the organic phase is washed with saturated aqueous NaCl solution. It is then concentrated and the residue is separated on silica gel (petroleum ether/AcOEt=1+1). The appropriate fractions crystallize from Et2O/petroleum ether. 230 mg of the title compound are obtained. MS:333.8 Rf =0.57 (petroleum ether/AcOEt=1+1)

1. stirringthe mixture is stirred again for 30 min
2. washthe organic phase is washed with saturated aqueous NaCl solution
3. concentrationIt is then concentrated
4. customthe residue is separated on silica gel (petroleum ether/AcOEt=1+1)
5. customThe appropriate fractions crystallize from Et2O/petroleum ether