摘要
以氯氯苄,三苯基膦和邻磺酸钠苯甲醛为原料,经Witting-Horner反应制得4-氯-二苯乙烯-2'-磺酸钠,然后在含Ni催化剂的作用下制得了荧光增白剂CBS[4,4'-双-2-(磺酸钠苯乙烯基)联苯].该工艺规避了联苯的氯甲基化过程,可减少有毒物质的排放量,为合成联苯类荧光增白剂提供了1种新方法.优化后的反应条件:中间体的合成温度为50℃,n(碱)∶n(三苯基膦)为1.1∶1.0;合成CBS反应温度为80℃,催化剂用量为5%.总收率可达64.9%以上.
p-Chlorobenzyl chloride, triphenylphosphine and Na o-benzaldehydesulfonate were used as raw materials for the synthesis of Na p-chlorostilbene-o'-sulfonate (I) by Wittig-Horner reaction. Fluorescent White- ning Agent CBS [p,p'-bis(o-sulfonylstyryl)biphenyl Na salt] was prepd. from I with Ni catalyst. This process avoided the course of biphenyl chlorormethylation, decreased the toxic substance effluents and supplied a new method for synthesis of biphenyl fluorescent whitening agents. The optimized reaction conditions were as follows: reaction temp. for I synthesis was 50 ℃, base ∶ triphosphine 1.1∶1.0 (mol ratio), reaction temp. for CBS sy- nthesis 80 ℃ and catalyst amt. 5%. The overall yield was over 64.9%.
出处
《印染助剂》
CAS
2005年第3期21-23,共3页
Textile Auxiliaries
关键词
荧光增白剂
磺酸
合成
氯苄
烯基
总收率
催化剂用量
新方法
原料
三苯基膦
fluorescent whitening agent
chlorostilbenesulfonate process
4,4'-bis(2-sulfonylstyryl)-biphenyl sodium salt
