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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)技术表征产物氘代率的方法
Deuterium acetaldehyde (CD3CDO) is prepared from heavy water (D2 O) and calcium carbide (CaC2). Deuterobenzene reacts with bromine and metallic magnesium to form deuterated phenylmagnesium bromide (C6D5MgBr). The CD3CDO was then subjected to Grignard reaction with C6D5MgBr and hydrolyzed with aqueous acidic heavy water to give a fully deuterated α-phenylethanol (C6D5-CDODCD3) with a deuteration rate xD ≈ 99% with a yield of 71.2% (calculated as deuterated bromobenzene ). The authors introduce the synthesis of C6D5-CDODCD3 using D2 O, CaC2 and C6D6 as raw materials and the method of characterizing the deuteration rate of the product by 1HNMR using the internal standard relative molarity calibration factor hydrogen nuclear magnetic resonance spectroscopy