Improved synthesis of N-n-butylthiophosphoric triamide
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    Abstract:

    The improved procedure for preparing N-n-butylthiophosphoric triamide was described. The important intermediate N-n-butylaminothiophosphoryl dichloride was synthesized from thiophosphoryl chloride reacted with n-butylamine in the tubular reactor, followed by ammonolysis by NH3 for about 3h to give the title compound. The overall yield was 65.1%. The structure of the product was characterized by IR、ESI - MS、1H - NMR and 13C - NMR. In the meanwhile, a few factors including molar ratio of raw materials, reaction temperature and residence time are investigated. And the optimum condition were: Molar ratio of thiophosphoryl chloride to n-butylamine is 1 : 1.5, residence time is 30s, tube length 14m, tube diameter 3mm, 28 ~ 30℃。

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History
  • Received:October 14,2011
  • Revised:October 23,2011
  • Adopted:November 01,2011
  • Online: December 26,2011
  • Published:
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