文章摘要
罗勇.稳定同位素标记D6-氯丙那林的合成[J].精细化工,2020,37(3):
稳定同位素标记D6-氯丙那林的合成
Synthesis of Isotope-labeled D6-Clorprenaline
投稿时间:2019-08-17  修订日期:2019-10-14
DOI:
中文关键词: D6-氯丙那林,同位素标记,合成,表征
英文关键词: D6-clorprenaline  isotope-labeled  synthesis  characterization
基金项目:上海市中央引导地方科技发展专项资金项目(YDZX20173100004528)
作者单位E-mail
罗勇 上海化工研究院 real-luoyong@hotmail.com 
摘要点击次数: 104
全文下载次数: 0
中文摘要:
      D6-氯丙那林的合成以邻氯苯乙酮和D6-丙酮为起始原料,邻氯苯乙酮与溴化铜通过溴化反应得到α-溴代邻氯苯乙酮,D6-丙酮经过还原、溴化、胺化、肼解、碱解得到D6-异丙胺,然后α-溴代邻氯苯乙酮和D6-异丙胺通过胺化、还原“一步法”合成得到稳定同位素标记的D6-氯丙那林,以投入的D6-异丙胺的物质的量计算产率为26.2%。目标产物结构经NMR、MS、HPLC和X-ray单晶衍射等表征确认,液相色谱纯度大于98%,液质丰度99.7% atom D,可作为内标试剂用于氯丙那林残留的检测。
英文摘要:
      D6-clorprenaline was synthesized with D6-acetone (99.9% atom D) and 2'-chloroacetophenone as starting materials. 2'-Chloroacetophenone is brominated by copper bromide to obtain 2-bromo-2'-chloroacetophenone. D6-isopropyl-amine was synthesized by reduction, bromination, amina-tion, hydrazinolysis and alkali hydrolysis reaction with D6-acetone. Then a one-pot method of amination and reduction was designed to synthesize D6-clorprenaline. The yield based on the amount of substance of D6-isopropyl-amine was 26.2%. The structure of target product was confirmed by NMR, MS, HPLC and X-ray crystal diffraction. Its chemical purity was higher than 98%, and isotopic abundance was 99.7% (atom D). The above compound could be used as an internal standard reagent for the determination of residual clorprenaline.
  查看/发表评论  下载PDF阅读器
关闭