4,4′-双(苯并口恶唑-2-基)二苯乙烯荧光增白剂(OB-1)的合成

Synthetic Process of Fluorescent Bleaching Agent 4,4′-Bis(benzoxazol-2-yl)stilbene OB-1

以对甲基苯甲酸及其乙酯为原料,经过三氧化铬在乙酐中的氧化反应、在氯苯溶剂中以氯化亚砜为氯化试剂的侧链氯化反应和亚磷酸三乙酯为乙基化试剂的酯化反应,再经两步缩合反应,合成了荧光增白剂4,4′ 双(苯并口恶唑 2 基)二苯乙烯(OB-1)。OB-1(由Ⅲ合成Ⅳ粗品)的收率由文献中平均90%提高到平均99%以上。通过对化合物的元素分析、红外光谱以及在DMF中紫外吸收光谱的测定,确定了目标产物的结构。经HPLC测定,w(OB-1)>99%。

With pmethylbenzoic acid and its ethyl ester as starting materials,the fluorescent bleaching agent 4,4′bis(benzoxazol2yl)stilbene(OB-1) was synthesized by oxidation with CrO3 in acetic anhydride,side chain chlorination with SOCl2 in chlorobenzene,esterification with triethyl phosphite and two steps of condensation reactions.The average yield of OB-1 was raised from average 90% in the literature to 99% and over.The objective product was characterized by elementary analysis,IR and ultraviolet absorption spectrometry in DMF.HPLC analysis proved that w(OB-1) was higher than 99%.