摘要
以乙醛酸、苯酚、氨基磺酸为原料,3-乙基苄基氯化铵为相转移催化剂,一步法合成了DL-对羟基苯甘氨酸。实验发现,晶体乙醛酸是适宜的合成原料。考察了原料配比、反应温度、催化剂用量、反应时间对产品收率的影响,确定了较佳反应条件为:n(乙醛酸):n(苯酚):n(氨基磺酸)=1:1.3:1.3,反应温度70℃,催化剂用量0.444 g,反应时间8 h。在该反应条件下,单程收率达70%以上,母液回收套用后总收率达75%以上。经高效液相色谱法测得产品纯度为99.1%,对产品结构进行了红外光谱表征。
DL - p - hydroxyphenylglycine was synthesized by one - step method using crystal glyoxylic acid, phenol and sulfamic acid as raw materials and benzyhriethylammonium chloride as phase transition catalyst. It was found that crystal glyoxylic acid was suitable raw material. Effects of some factors such as molar ratio of reactants, reaction temperature, dosage of catalyst and reaction time on reaction were examined. The optimum reaction conditions were as follows ： n （ glyoxylic acid） ： n （phenol） ： n （ sulfamic acid） = 1 ： 1.3 ： 1.3, reaction temperature 70 ℃, dosage of catalyst 0.444 g and reaction time 8h. Under these conditions,the single yield of product was above 70% ,the yield was above 75 % by recycling the mother liquid. The purity of product was 99.1% and the structure of product was characterized by FT - IR.
出处
《精细石油化工进展》
CAS
2007年第11期20-23,共4页
Advances in Fine Petrochemicals
关键词
晶体乙醛酸
合成
DL-对羟基苯甘氨酸
crystal glyoxylic acid, synthesis, DL - p - hydroxyphenylglycine
