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Chemical Structure| 1227002-36-9 Chemical Structure| 1227002-36-9

Structure of 1227002-36-9

Chemical Structure| 1227002-36-9

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Product Details of [ 1227002-36-9 ]

CAS No. :1227002-36-9
Formula : C8H9F3N2O3
M.W : 238.16
SMILES Code : O=C(C1=CC(OCC(F)(F)F)=NN1C)OC
MDL No. :N/A
Boiling Point : No data available

Safety of [ 1227002-36-9 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319
Precautionary Statements:P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Application In Synthesis of [ 1227002-36-9 ]

* 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.

  • Downstream synthetic route of [ 1227002-36-9 ]

[ 1227002-36-9 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 433-06-7 ]
  • [ 52867-42-2 ]
  • [ 1227002-36-9 ]
YieldReaction ConditionsOperation in experiment
50% With potassium carbonate; In water; N,N-dimethyl-formamide; Methyl 1-methyl-3-(2,2,2-trifluoroethoxy)-1H-pyrazole-5-carboxylate A solution of 200 mg (1.28 mmol) of methyl 3-hydroxy-1-methyl-5-pyrazolecarboxylate (for preparation see above) in 10 ml of N,N-dimethylformamide is admixed with 254 mg (2.56 mmol) of 2,2,2-trifluoroethyl-4-methylbenzenesulphonate and 138 mg (2.56 mmol) of potassium carbonate and the reaction mixture is heated at 100 C. for five hours and afterstirred at room temperature for two days. The reaction mixture is added to water and extracted several times with ethyl acetate. The organic phase is dried over sodium sulphate, filtered and concentrated by evaporation in vacuo on a rotary evaporator. This gives 500 mg of methyl 1-methyl-3-(2,2,2-trifluoroethoxy)-1H-pyrazole-5-carboxylate (50% strength, 82%). 1H-NMR (400 MHz, d6-DMSO): delta=6.41 (s, 1H), 4.77 (m, 2H), 3.94 (s, 3H), 3.83 (s, 3H) ppm. HPLC-MS: log P=2.61; mass (m/z)=239 [M+H]+.
  • 2
  • [ 353-83-3 ]
  • [ 52867-42-2 ]
  • [ 1227002-36-9 ]
YieldReaction ConditionsOperation in experiment
16% With sodium hydride; In N,N-dimethyl-formamide; mineral oil; at 100℃; for 2.16667h;Sealed tube; Cooling with ice; methyl 5-hydroxy-2-methyl-pyrazole-3-carboxylate (2.7 g, 17.0 mmol) and 2-iodo-l,l,l- trifluoroethane (2.1 mL, 21 mmol) were dissolved in anhydrous DMF (20 mL). The reaction was cooled in an ice bath prior to addition of sodium hydride (1.20 g, 29 mmol, 60 mass% in mineral oil) portion- wise over 10 min. Upon completion of addition, the reaction was sealed and heated to 100 C with stirring for 2 h. The reaction was diluted with water (20 mL) and extracted with EtOAc (3 x 20 mL). The organic layer was dried over Na2S04 and concentrated in vacuo. The crude product was purified by column chromatography eluting with a 0-50% gradient of EtOAc in isohexane. Product-containing fractions were combined and concentrated to afford the title compound (660 mg, 16% Yield). dH (300 MHz, Chloroform-cf) 6.25 (s, 1H), 4.55 (q, J = 8.4 Hz, 2H), 4.03 (s, 3H), 3.87 (s, 3H).
 

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