反应详情

温度

5 °C

Methyl 4-{[2-(dimethylamino)-2-oxoethyl]oxy}-3-(methyloxy)benzoate (for a preparation see Intermediate 22) (1.4 g, 5.2 mmol) was dissolved in THF (50 ml) and cooled in an ice-bath under nitrogen. The mixture was then treated cautiously with 1M ether solution of lithium aluminium hydride (5.5 mL) and the mixture was stirred at 5° C. allowing to warm to RT overnight. The reaction mixture was quenched by cautious addition of aq. saturated NaHCO3 solution (1 mL), followed by MgSO4 (2 g) and stirring for 30 min. The solids were removed by filtration, washed with ethyl acetate, and the filtrate was evaporated to give the title compound (1.18 g, 100%) as a yellow oil: LCMS (System A) RT=0.34 min, ES+ve m/z 226 (M+H)+.

1. temperaturecooled in an ice-bath under nitrogen
2. temperatureto warm to RT overnight
3. customThe reaction mixture was quenched by cautious addition of aq. saturated NaHCO3 solution (1 mL)
4. stirringstirring for 30 min
5. customThe solids were removed by filtration
6. washwashed with ethyl acetate
7. customthe filtrate was evaporated