Synthesis of Labeled of Tulobuterol - D9
DOI:
CSTR:
Author:
Affiliation:

Clc Number:

O628.2;TQ 421.6

Fund Project:

  • Article
  • |
  • Figures
  • |
  • Metrics
  • |
  • Reference
  • |
  • Related
  • |
  • Cited by
  • |
  • Materials
  • |
  • Comments
    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.

    Reference
    Related
    Cited by
Get Citation
Share
Article Metrics
  • Abstract:
  • PDF:
  • HTML:
  • Cited by:
History
  • Received:November 14,2014
  • Revised:February 02,2015
  • Adopted:February 03,2015
  • Online: April 08,2015
  • Published:
Article QR Code