反应详情

温度

-55 °C

14.8 g lithium aluminium hydride were weighed under N2 atmosphere into a round-bottomed flask. The substance was cooled down to −55° C. and 150 ml ether was added dropwise. The suspension was allowed to stir; then 30 g 4-Morpholin-4-yl-butyronitrile were dissolved in 200 ml ether and the solution was added dropwise to the reaction mixture. Again 200 ml ether were added to the mixture and the reaction was stirred at room temperature overnight. At the next day the mixture was cooled down to less than 10° C. and 35 ml H2O were added carefully. After five hours the mixture was fritted and the residue was washed with 300 ml ether. The filtrate was dried, concentrated and finally distilled under vacuum. The product fractions were collected at 74-78° C. and 2.1-1.6 Torr. The purity of the colourless oil was judged by gas chromatography, GC-MS and 1H-NMR.

1. additionthe solution was added dropwise to the reaction mixture
2. stirringthe reaction was stirred at room temperature overnight
3. temperatureAt the next day the mixture was cooled down to less than 10° C.
4. washthe residue was washed with 300 ml ether
5. customThe filtrate was dried
6. concentrationconcentrated
7. distillationfinally distilled under vacuum
8. customThe product fractions were collected at 74-78° C.