反应 #3752301
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06570031B1
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 20 g (0.1 mol) of N,N-dimethylundecylamine were added in portions with stirring to 14.8 g (0.15 mol) of concentrated hydrochloric acid (37 wt. %). After the exothermic reaction (up to approx. 35° C.), the highly viscous mixture was diluted with 5 ml of concentrated hydrochloric acid and 5 ml of water, stirred for a further 2 hours and finally left to stand overnight. The aqueous phase was then extracted with 80 ml of methylene chloride, the organic phase dried with sodium sulfate and the solvent removed under a vacuum. In order to remove any traces of water, the residue was resuspended in 80 ml of toluene and concentrated under a vacuum and the operation was then repeated in 100 ml of hexane. Once the solvent had again been removed by distillation under a vacuum, N,N-dimethylundecylammonium hydrochloride was obtained as a colourless solid. After the exothermic reaction (up to approx. 35° C.) finally left to stand overnight The aqueous phase was then extracted with 80 ml of methylene chloride the organic phase dried with sodium sulfate the solvent removed under a vacuum In order to remove any traces of water concentrated under a vacuum Once the solvent had again been removed by distillation under a vacuum
来源 ID: ord-9557876d2b5b4bceb9f3ee2ecbd91745