2-羟基-4-苄氧基二苯甲酮的合成

以间苯二酚、三氯甲苯和苄基氯为原料,通过两步反应合成2-羟基-4-苄氧基二苯甲酮。第一步采用以间苯二酚和三氯甲苯为原料,在十六烷基三甲基溴化铵作为相转移剂时,合成了中间体2,4-二羟基二苯甲酮,其反应的适宜条件为:反应原料n(三氯甲苯)/n(间苯二酚)比为1.4、滴加温度为60℃、反应温度为70℃、反应时间为0.5 h和催化剂用量为3.0 g/mol(以间苯二酚计),产品收率在95%以上。第二步采用以中间体2,4-二羟基二苯甲酮和苄基氯为原料,合成最终产物2-羟基-4-苄氧基二苯甲酮,结果表明,反应原料n(苄基氯)/n(2,4-二羟基二苯甲酮)比为1.0、Na2CO3为106.0 g/mol(以2,4-二羟基二苯甲酮计)、环已酮为40 mL和反应时间为6 h,产率在77%以上。得到的中间体和产物通过红外光谱、元素分析和1H-NMR进行表征。

Synthesis of 2-Hydroxy-4-Benzyloxybenzophenone

2-Hydroxy-4-benzyloxybenzophenone was synthesized from resorein, trichlorotoluene and benzyl chloride as the raw material by two steps. In the first step, resorein and trichlorotoluenc were used as raw material to synthesize the intermediate product of 2,4-dihydroxybenzophenone, hexadecyl trimethyl ammonium bromide as phase transfer catalyst. The optimum condition for synthesis was as follows： molar ratio of trichlorotoluene to resorcin is 1.4, dropping temperature is 60 ℃, reaction temperature is 70 ℃, reaction time is 0.5 h,dosage of catalyst is 3.0 g/mol（referred to resorcin）. Under this condition, the yield of the product can be up to 95%. In the second step, the intermediate product of 2,4-dihydroxybenzophenone and benzyl chloride were used as raw material to synthesize the final product of 2-hydroxy-4-benzyloxybenzophenone. The experimental results show that the yield of the product can be above 77% when the material ratio of benzyl chloride to 2, 4-dihydroxybenzophenone is 1.0, Na2CO3 is 106.0 g/mol （referred to 2, 4- dihydroxybeuzophenone） ,cyclohexanone is 40 mL,and reaction time is 6 h. The intermediate product and the final product were characterized by infrared spectrum analysis, elementary analysis and ^1H-NMR.