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Chemical Structure| 454-31-9 Chemical Structure| 454-31-9

Structure of 454-31-9

Chemical Structure| 454-31-9

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Product Details of [ 454-31-9 ]

CAS No. :454-31-9
Formula : C4H6F2O2
M.W : 124.09
SMILES Code : O=C(OCC)C(F)F
MDL No. :MFCD00013578
InChI Key :GZKHDVAKKLTJPO-UHFFFAOYSA-N
Pubchem ID :9961

Safety of [ 454-31-9 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H226-H314
Precautionary Statements:P210-P233-P240-P241-P242-P243-P264-P280-P301+P330+P331-P303+P361+P353-P304+P340+P310-P305+P351+P338+P310-P363-P370+P378-P403+P235-P405-P501
Class:3(8)
UN#:2924
Packing Group:

Application In Synthesis of [ 454-31-9 ]

* 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 [ 454-31-9 ]

[ 454-31-9 ] Synthesis Path-Downstream   1~6

  • 1
  • [ 383-62-0 ]
  • [ 454-31-9 ]
YieldReaction ConditionsOperation in experiment
>= 75% With palladium on activated charcoal; hydrogen; triethylamine; In ethanol; at 30℃; under 750.075 - 3000.3 Torr; 1 part of <strong>[383-62-0]ethyl difluorochloroacetate</strong>Triethylamine 0.5 part5 parts of ethanolPalladium on carbon 0.002 partsThe preparation of the above ethyl ethyl difluoroacetate comprises the following steps:(1) 1 part of <strong>[383-62-0]ethyl difluorochloroacetate</strong>, 0.5 part of triethylamine, 5 parts of solvent ethanol and 0.002 part of palladium on carbon were successively charged in a high pressure reactor;(2) the first nitrogen replacement reactor air at least 3 times, and then replaced with hydrogen at least 3 times, slowly warming to 30 C, then the pressure in the O.IMPa around;(3) and then slowly through the hydrogen to the pressure of 0.4MPa to carry out hydrogenation reaction, when the pressure inside the kettle down to O.IMPa, again through the hydrogen to the kettle pressure 0.4MPa;(4) Repeat step (3) several times until the pot pressure is no longer falling and the reaction is over;(5) sample analysis of the reactants in the raw materials ethyl dichloroacetate content;(6) Distillation: The product obtained in step (4) is subjected to atmospheric distillation in a glass bottle, and the product is separated from ethyl difluoroacetate and solvent ethanol. The bottoms are filtered and washed with water to recover the catalyst. In the next reaction.
  • 2
  • [ 454-31-9 ]
  • [ 2932-65-2 ]
  • 4,4-difluoro-1-(4-propyl-phenyl)-butane-1,3-dione [ No CAS ]
  • 3
  • [ 454-31-9 ]
  • [ 2923-66-2 ]
  • (Z)-4-(3-Chloro-4-fluoro-phenyl)-1,1-difluoro-4-hydroxy-but-3-en-2-one [ No CAS ]
  • 4
  • [ 383-62-0 ]
  • [ 381-73-7 ]
  • [ 454-31-9 ]
  • [ 76-04-0 ]
  • 5
  • [ 313735-62-5 ]
  • [ 454-31-9 ]
  • 2,2-difluoro-1-(1-isopropyl-1H-pyrazol-4-yl)ethan-1-one [ No CAS ]
YieldReaction ConditionsOperation in experiment
48% 4-bromo-1-(isopropyl)-1H-pyrazole 11d (200 mg, 1.06 mmol) was dissolved in dry THF (6 mL) at -78 Cunder nitrogen and was stirred for 10 min. n-BuLi (2.5 M in hexanes, 0.44 mL, 1.11 mmol) was added drop wise to the solution was stirred for 2 h at -78 C. After two hours, ethyl difluoroacetate (0.11 mL, 1.27 mmol) was added drop wise and stirred for 10 min at -78 C uponwhich the mixture was then quenched with NH4Cl (20 mL) and warmed to room temp. Themixture was then extracted with ether (50 mL), and dried over MgSO4. After concentration invacuo (note: remove shortly after the ether is removed, because the compound is quite volatile),the residue was purified with flash chromatography over silica gel (hexane: ethyl acetate =80:20) to yield the product as a clear oil in 48% yield (0.1 g).
  • 6
  • [ 383-62-0 ]
  • [ 359-13-7 ]
  • [ 454-31-9 ]
YieldReaction ConditionsOperation in experiment
With palladium on activated charcoal; hydrogen; triethylamine; In ethanol; at 45℃; under 7500.75 - 30003 Torr; for 5h; Take a dry and clean reactor, add the magnet. Use the electronic balance to weigh 0.1-lgPd / C on the weighing paper. 30 g of ethanol, 10 g of <strong>[383-62-0]ethyl difluorochloroacetate</strong> and 2.8 g of triethylamine were weighed into the reaction kettle, and the kettle was screwed. Fill 4MPa of hydrogen and use the instrument to check whether the kettle leak, do not leak is deflated, continue to repeat three times, the last inflated to 1. OMPa. And then into the 45 C silicone bath for 5h, after the time, come up to cool down to about 40 C temperature, deflate, unscrew the kettle cover, with dropper sampling, chromatographic analysis, the results of the table 1.
 

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