Synthesis of Thiocarbamates by Carbonylation of Aromatic Nitro-compounds in Ionic Liquid
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O 625. 4 ; TQ 244. 1

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    Abstract:

    A effective carbonylation of aromatic nitro-compounds with thiols or thiophenols catalyzed by Pd-Fe/TiO2 in ionic liquid 1-butyl-3-methylimidazolium hexafluorophosphate ([bmim]PF6) was studied. The influences of reaction medium, Pd and Fe loading, molar ratio of nitro-compound to thiols, catalyst dosage and reaction temperature on the carbonylation reactions were investigated. Pd-Fe/TiO2 catalyst with mass fraction of Pd 0.5% and mass fraction of Fe 0.3% exhibits high activity for carbonylation reactions. The carbonylation of some aromatic nitro-compounds with thiols or thiophenols catalyzed by Pd-Fe/TiO2 in ionic liquid can proceed well to thiocarbamates in good yield under the conditions of nitro-compound 10 mmol, thiols or thiophenols 11 mmol, catalyst dosage 36 mg, ionic liquid 10 mL, CO pressure 0.1 MPa, reaction temperature 30 ℃, reaction time 3~8 h. The catalyst and ionic liquid can be reused for six times without significant decrease in the yield of thiocarbamates.

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History
  • Received:October 11,2010
  • Revised:November 17,2010
  • Adopted:December 02,2010
  • Online: January 10,2011
  • Published:
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