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研究了以对甲酚、溴和过氧化氢等为主要原料 ,经过溴化、甲氧基化和氧化反应合成香兰素的工艺。 0 .6mol溴和 1 .0 mol过氧化氢在 1 0℃ ,4 h内滴加到 1 .5mol对甲酚和 1 50 m L甲醇的混合物中 ,得到 1 80 g 2 -溴对甲酚 ( ) ;( )与甲醇钠在 1 45℃和 1 .0～ 1 .2 MPa条件下反应 2 .5h生成 1 2 4 g2 -甲氧基对甲酚 ( ) ;( )在乙酸钴存在下 ,用空气氧化得到 4 4g香兰素 ,总收率为 70 %。
The process of synthesizing vanillin by bromination, methoxylation and oxidation with p-cresol, bromine and hydrogen peroxide as the main raw materials was studied. 0.6 mol of bromine and 1.0 mol of hydrogen peroxide were added dropwise to a mixture of 1.5 mol of p-cresol and 150 mL of methanol at 0 ° C for 4 h to give 180 g of 2-bromo-p-cresol ); () With sodium methoxide at 1 45 ℃ and 1. 0 ~ 1. 2 MPa reaction conditions 2.5 hours to produce 1 2 4 g2 - methoxy p-cresol (); () in the presence of cobalt acetate with Air oxidation gave 4 4g vanillin in a total yield of 70%.