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目的对4-O-丁香树脂酚的合成工艺进行改进。方法以丁香醛为原料,与丙二酸进行Knovevenagel缩合得到芥子酸,再将芥子酸用乙醇进行乙酯化得到不饱和酯、以Al H(Bu-i)2为还原剂将酯还原为芥子醇、芥子醇在光照通入空气的条件下经过氧化偶联得4-O-丁香树脂酚。结果芥子酸的合成中,将催化剂哌啶换成相同碱性的四氢吡咯,在大幅度缩短反应时间的条件下,该步反应产率也明显提高;酯的还原中将溶解性较差的氢化锂铝换成溶解性好的二异丁基氢化铝,以甲苯为溶剂进行还原,收率明显提高,且无需后处理,可直接投入下一步反应,总收率约51%。结论该方法工艺简单,有产业化前景。
Objective To improve the synthesis of 4-O-clove resin phenol. Methods Syringatoaldehyde was used as a raw material, Knovevenagel condensation with malonic acid was carried out to obtain sinapic acid, and then erucic acid was ethyl esterified with ethanol to obtain unsaturated ester. Al H (Bu-i) 2 was used as reducing agent to reduce ester to mustard The alcohol, mustard alcohol is oxidatively coupled to 4-O-clove resin phenol under light-on conditions. The results of the synthesis of erucic acid, the catalyst piperidine replaced by the same basic pyrrole, in a substantial reduction in reaction time conditions, the reaction rate was significantly improved; ester will be less soluble in the reduction of the reduction Lithium aluminum hydride into a good solubility of diisobutylaluminum hydride, toluene as a solvent for reduction, the yield was significantly improved, and without post-treatment, can be directly into the next reaction, the total yield of about 51%. Conclusion The method is simple, with industrial prospects.