没食子酸制备三乙酰基没食子酰氯工艺研究

Study on the preparation of trisacetyl-galloylchloride from gallic acid

以没食子酸与乙酸酐合成三乙酰没食子酸(TAGA),进而以N,N-二甲基甲酰胺(DMF)为催化剂,与SOCl2酰氯化反应合成三乙酰没食子酰氯(TAGC),考察了溶剂、反应物配比、催化剂加入量、浴温及反应时间对产率的影响。结果表明,二氯甲烷反应效果最好,优化工艺条件为:TAGA与SOCl2摩尔比为1∶3,催化剂加入量1.2%,浴温60℃,反应时间3 h。在此条件下,TAGC产率可达92.9%。

Synthetic technique of the trisacetyl-galloylchloride（TAGC）was studied,and TAGC was synthesized using dimethylformamide（DMF）as catalyst,SOCl2 and the trisacetylgallic acid（TAGA）as materials,the latter was the reactant of gallic acid and acetic anhydride.The influence of reaction conditions such as solvents,catalyst dosage,reaction temperature and time on the yield was discussed.The results showed that the best reaction effect was using dichloromethane as solvent,the optimum technological conditions were as follows：n（TAGA） ∶n（SOCl2）=1 ∶3,catalyst dosage 1.2%,reaction temperature 60 ℃ and reaction time 3 h.The yield of TAGC could reach 92.9%,and the struture of the obtained material was characterized by IR.