格林尼亚反应合成全氘代-α-苯乙醇  

Synthesis of Perdeutero-α-phenylethanol by Grignard Reaction

作　　者：张林[1] 谢如刚[2] 刘维铭[2] 高文德[2] 

机构地区：[1]中国工程物理研究院激光聚变研究中心,四川绵阳621900 [2]四川大学化学系,四川成都610064

出　　处：《精细化工》2001年第10期614-616,共3页Fine Chemicals

基　　金：国家高新技术 86 3 -4 16 -3专题资助项目~~

摘　　要：以重水 (D2 O)及电石 (CaC2 )为原料 ,先制得氘代乙醛 (CD3CDO) ;氘代苯则与溴和金属镁反应生成氘代苯基溴化镁 (C6D5MgBr)。CD3CDO再与C6D5MgBr进行格林尼亚反应 ,并用酸性重水溶液水解 ,最终制得氘代率xD≈ 99%的全氘代 α 苯乙醇 (C6D5—CDODCD3) ,产率 71.2 % (以氘代溴苯计 )。作者介绍了以D2 O、CaC2 及C6D6为原料制备C6D5—CDODCD3 的合成工艺及采用内标相对摩尔校正因子氢核磁共振波谱 (1HNMR)Perdeutero α phenylethanol (C 6D 5-CDODCD 3) was synthesized by Grignard reaction.Heavy water(D 2O)reacted with calcium carbide to give acetaldehyde d 4 (CD 3CDO).Deuterated benzene reacted successively with bromine and magnesium to produce phenyl d 5 magnesium bromide (C 6D 5MgBr).CD 3CDO reacted with C 6D 5MgBr and then gave C 6D 5-CDODCD 3 by acidic heavy water hydrolysis.The yield of C 6D 5-CDODCD 3 is 71.2% (based on C 6D 5Br used) and the deuterium content χ D was about 99% as measured by 1 HNMR.The methods of synthesis and determination of deuterium content for C 6D 5-CDODCD 3 were described in this paper.

关 键 词：格林尼亚反应 氚代-α-苯乙醇 氚代率 表征 合成 

分 类 号：TQ243.4[化学工程—有机化工]