反应详情

25 g (84.2 mmol) of 3-iodobenzyl bromide are added to a solution of 24.3 g (88.4 mmol) of diethyl [(tert-butoxycarbonyl)amino]malonate and 3.7 g (92.6 mmol) of sodium hydride in 300 ml of DMF while cooling in ice. After stirring the mixture at RT for 4 h, 5 ml of water are added cautiously while cooling in ice. The mixture is extracted several times with ethyl acetate, and the combined organic phases are washed with a saturated sodium chloride solution and water, dried over magnesium sulfate and concentrated in vacuo. The crude product is dried under high vacuum.

1. temperaturewhile cooling in ice
2. temperaturewhile cooling in ice
3. extractionThe mixture is extracted several times with ethyl acetate
4. washthe combined organic phases are washed with a saturated sodium chloride solution and water
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated in vacuo
7. dry with materialThe crude product is dried under high vacuum