摘要
以苯乙酮和澳代苯为原料,通过格氏反应先制得1,1-二苯基乙醇(1),收率为91.3%;(1)经脱水和氯甲基化得到1,1-二苯基-3-氯丙烯(2),收率为92.9%;(2)再与二苯甲酮衍生物经格氏反应制得了1,1,4,4-四苯基-1,3-丁二烯衍生物(3a)和(3b),收率高于54.0%,并对各步合成的工艺条件进行了研究。HPLC测得(3a)和(3b)质量分数均高于99.0%。通过紫外光谱、红外光谱、质谱、1^H NMR和元素分析对产物的组成和结构进行了鉴定。
1,1-diphenylethanol(1) was firstly prepared by the Grignard reaction of bromobenzene and acetophenone with the yield of 91.3%, and then via the dehydration and chloromethylation of which, the 1,1-diphenyl-3-chlompropylene (2) was got, with the yield of 92.9%. At last, the 1,1,4,4-tetraphenyl-1,3-butadiene derivatives (3a) and (3b) were synthesized by the Grignard reaction of (2) and benzophenone derivatives, with the yields being higher than 54.0%. The synthesizing requirements of all the steps were studied. The mass fraction of (3a) and (3b) measured by HPLC were higher than 99.0%. And the composition and the structure of the products were measured by UV, IR, MS, 1^H NMR and elemental analysis.
出处
《高技术通讯》
CAS
CSCD
北大核心
2006年第12期1269-1272,共4页
Chinese High Technology Letters
基金
863计划(2002AA325050)和天津市应用基础研究计划(06YFJZJC01600)重点资助项目.