反应详情

A solution of 31.44 g allyl-carbamic acid tert-butyl ester (200 mmol) in 300 ml DMF and 30 ml dry THF is treated with 12 g (300 mmol) NaH (60% suspension in mineral oil). The temperature is kept below 40° C. with an cold water bath. When the development of hydrogen gas ceased the reaction mixture is treated, under ice cooling, with 24 ml (300 mmol) ethyl iodide. After 16 h the mixture is diluted with 1 L water and extracted with TBME. The organic layer is washed extensively with water, concentrated under reduced pressure and distilled at 0.3 mmHg, bp. 38-39°, to yield the allyl-ethyl-carbamic acid tert-butyl ester.

1. customThe temperature is kept below 40° C. with an cold water bath
2. extractionextracted with TBME
3. washThe organic layer is washed extensively with water
4. concentrationconcentrated under reduced pressure
5. distillationdistilled at 0.3 mmHg, bp. 38-39°