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Chemical Structure| 153085-15-5 Chemical Structure| 153085-15-5

Structure of 153085-15-5

Chemical Structure| 153085-15-5

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Product Details of [ 153085-15-5 ]

CAS No. :153085-15-5
Formula : C5H5F3N2
M.W : 150.10
SMILES Code : FC(C1=CC=NN1C)(F)F
MDL No. :MFCD16619801

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Application In Synthesis of [ 153085-15-5 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Upstream synthesis route of [ 153085-15-5 ]
  • Downstream synthetic route of [ 153085-15-5 ]

[ 153085-15-5 ] Synthesis Path-Upstream   1~3

  • 1
  • [ 59938-06-6 ]
  • [ 60-34-4 ]
  • [ 153085-15-5 ]
  • [ 154471-65-5 ]
YieldReaction ConditionsOperation in experiment
24 g at 55℃; for 20 h; Cooling with ice ETFBO (270 g, 1.61 mol, 1.00 eq) was dissolved in methanol (750 mL). The solution was cooled in an ice/water-bath and methyl hydrazine (88.3 mL, 77.7 g, 1.69 mol, 1.05 eq) was added dropwise within 20 minutes. The mixture was heated to 55°C and stirred at this temperature for 20 h in dry air (drying tube). Successively the solvent was removed and the residue distilled under vacuum : 1st Fraction : 150 mbar, 130°C bath temperature, 73~85°C, mixture of isomers, 129 g.2nd Fraction : 70 mbar, 150°C bath temperature, 75~85°C, 1-methyl-3-(trifluoromethyl)-1H-pyrazole, 24 g. Overall yield : 153 g (1.02 mol) 63 percent.
References: [1] Patent: EP2662359, 2013, A1, . Location in patent: Page/Page column 6; 10.
  • 2
  • [ 59938-06-6 ]
  • [ 60-34-4 ]
  • [ 153085-15-5 ]
  • [ 154471-65-5 ]
YieldReaction ConditionsOperation in experiment
24 g at 55℃; for 20 h; Cooling with ice The solution was cooled in an ice/water-bath and methyl hydrazine (88.3 mL, 77.7 g, 1.69 mol, 1.05 eq) was added dropwise within 20 minutes. The mixture was heated to 55°C and stirred at this temperature for 20 h in dry air (drying tube). Successively the solvent was removed and the residue distilled under vacuum : 1st Fraction : 150 mbar, 130°C bath temperature, 73~85°C, mixture of isomers, 129 g. 2nd Fraction : 70 mbar, 150°C bath temperature, 75-85 °C, l-methyl-3-(trifluoro- methyl)-lH-pyrazole, 24 g. Overall yield : 153 g (1.02 mol) 63 percent.
References: [1] Patent: WO2013/167586, 2013, A1, . Location in patent: Page/Page column 10.
  • 3
  • [ 59938-06-6 ]
  • [ 60-34-4 ]
  • [ 153085-15-5 ]
  • [ 154471-65-5 ]
  • [ 272442-83-8 ]
References: [1] Journal of Heterocyclic Chemistry, 2003, vol. 40, # 6, p. 1087 - 1089.
 

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