稳定同位素标记妥布特罗-D9的合成
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O628.2;TQ 421.6

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科技部专制院所专项(No.2014EG116258 )和科技部十二五重点支撑计划(No. 2012BAK25B03-15)资助项目


Synthesis of Labeled of Tulobuterol - D9
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    摘要:

    :以自制的叔丁胺-D9为同位素标记前体,以邻氯苯乙酮为起始原料,经溴化后,再与叔丁胺- D9经胺化、硼氢化钠还原后得到稳定同位素标记的布特罗-D9。采用均匀设计法对胺化步骤进行研究,实验数据通过多元回归分析,得出了优化的工艺条件:反应温度59 ℃,反应时间5 h,溶剂量为25 mL,n(溴代酮): n(叔丁胺- D9)为1 : 2。目标产物结构经质谱(MS)和核磁(NMR)、高效液相色谱(HPLC)等仪器表征确认,化学纯度高于98.0 %,同位素丰度高于97.5 %(atom D),可作为食品安全领域检测用同位素内标试剂。

    Abstract:

    This paper presents an efficient synthesis of tulobuterol-D9 with self-made tert-butylamine-D9 as the labeled precursor. Tulobuterol-D9 was synthesized from O-chloroacetophenone as the starting material by bromination with CuBr2, amination with tert-butylamine-D9, reduction with NaBH4. Uniform design method was used to study the effects of the process conditions and experiment data was analyzed by quadratic polynomial regression. The optimized reaction parameters were: reaction temperature is 59 ℃, reaction time is 5 h, dosage of solvent is 25 mL, the molar ratio for bromoacetophenone and t-butylamine-D9 is 1:2. As-synthesized product was confirmed by MS, NMR and HPLC to be target compound. Its chemical purities is higher than 98.0 % and isotopic enrichment is higher than 97.5 %(atom D). The above compound could be used as internal standard in the field of food safety.

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罗勇.稳定同位素标记妥布特罗-D9的合成[J].精细化工,2015,32(5):

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  • 收稿日期:2014-11-14
  • 最后修改日期:2015-02-02
  • 录用日期:2015-02-03
  • 在线发布日期: 2015-04-08
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