Abstract:
In order to launch a new tobacco flavor,the industrial synthesis of 2,5-deoxyfructosazine(2,5-DOF),2-(tetrahydroxybutyl)-5-(2,3,4-trihydroxybutyl)-pyrazine,under a basic condition with glycosamine hydrochloride as an initial material and boric acid compounds as catalyst,was studied including reaction process and conditions,separation means and technical control.The synthesis product was characterized by element analysis,mass spectrometry,IR,
1H NMR,and
13C NMR,and its solubility and melt point were tested as well.The results showed that:1) boric acid was a preferable catalyst;2) the preferable mole ratio of glucosamine hydrochloride to boric acid and sodium hydroxide was 1:2.5:2.5;3) it was preferable to separete inorganic salts from reaction solution with nanofiltration membrane M150,and monitor the membrane separation with a hand-held conductivity meter;4)2,5-DOF was slightly soluble in methanol,acetone,and isopropyl alcohol,with a solubility of below 3 mg/mL generally,insoluble in propylene glycol,and its solubility in mixture of alcohol/water increased with the increase of the water proportion,and 5) the synthesis product was the target product,2,5-DOF,synthesis yield was 58.6% with purity of 97% and higher.