preparation | The tert-valeramide was first reduced with lithium aluminum tetrahydro. Tetrahydrofuran or 2-methyltetrahydrofuran can be selected as the reaction solvent, and the reaction conditions are consistent, but from the viewpoint of cost, tetrahydrofuran is preferred as the solvent; Tetrahydrolithium aluminum is used as the reduction reagent, usually 1 equivalent is used, if the reaction is less than 1 equivalent, the reaction is incomplete; The Exotherm is strongly exothermic when the material is added, and the reaction temperature can be controlled to not exceed 60 ° C. Considering the safe operation of the plant, preferably, the reaction temperature is controlled not to exceed 25 ° C, and then the reaction is maintained for 2 to 3 hours; The reaction can be quenched by 10% ~ 20% sodium hydroxide solution, and the higher the concentration of sodium hydroxide solution during quenching, the stronger the exotherm, the thicker the reaction solution, so it is preferable to use 10% sodium hydroxide solution while controlling the quenching temperature not to exceed 25 ° C.; The reaction solution is stirred for 1 hour after quenching to ensure sufficient reaction. The reaction solution was then filtered to obtain a tetrahydrofuran solution of crude pentylamine. This is followed by reaction with hydrochloric acid to form pentylamine hydrochloride. |