6-氨基-2-羟甲基正己烷- 1 -醇

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 6 g of diethyl 2-(3-cyanopropyl)malonate are added dropwise, at -10° C., to a suspension of 3 g of LiAlH4 in 100 ml of dry diethyl ether under N2. The mixture is slowly warmed to room temperature and then refluxed for 3 h. After renewed cooling to -10° C., the excess hydride is decomposed with water. The precipitate is removed on a frit and washed several times with diethyl ether. The ether solution is dried over MgSO4, filtered and evaporated in a rotary evaporator. Yield 0.66 g of 2-(4-aminobutyl)-1,3-propanediol, detectable in the 1H NMR and by C and H analysis. Glassy solid, melting point 126° C. (honey-like above 60° C.). refluxed for 3 h After renewed cooling to -10° C. The precipitate is removed on a frit washed several times with diethyl ether The ether solution is dried over MgSO4 filtered evaporated in a rotary evaporator Glassy solid, melting point 126° C. (honey-like above 60° C.)