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Chemical Structure| 2063-17-4 Chemical Structure| 2063-17-4

Structure of 2063-17-4

Chemical Structure| 2063-17-4

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Product Details of [ 2063-17-4 ]

CAS No. :2063-17-4
Formula : C6H7ClF2O3
M.W : 200.57
SMILES Code : O=C(OCC)CC(C(F)(Cl)F)=O
MDL No. :MFCD06656424

Safety of [ 2063-17-4 ]

Application In Synthesis of [ 2063-17-4 ]

* 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 [ 2063-17-4 ]

[ 2063-17-4 ] Synthesis Path-Downstream   1~4

  • 1
  • [ 2063-17-4 ]
  • [ 4922-98-9 ]
  • [ 1227418-25-8 ]
YieldReaction ConditionsOperation in experiment
In ISOPROPYLAMIDE; at 180℃; for 0.333333h;Microwave irradiation; Example 38; STEP A; To the solution of 3-phenyl-1H-1 ,2,4-triazol-5-amine (32 mg, 0.2 mmol) in DMA (0.5 ml_) was added ethyl 4-chloro-4,4-difluoro-3-oxobutanoate (40 mg, 0.2 mmol). The reaction mixture was stirred in microwave at 180 0C for 20 minutes, and then cooled to room temperature. The product, compound 38-1 , was purified by reverse phase HPLC.
  • 2
  • [ 383-62-0 ]
  • [ 141-78-6 ]
  • 4-chloro-4,4-difluoro-3,3-dihydroxy-butyric acid ethyl ester [ No CAS ]
  • [ 2063-17-4 ]
  • 3
  • [ 2063-17-4 ]
  • [ 76606-39-8 ]
  • [ 1350908-61-0 ]
  • 4
  • [ 383-62-0 ]
  • [ 141-78-6 ]
  • [ 2063-17-4 ]
YieldReaction ConditionsOperation in experiment
61% With n-butyllithium; diisopropylamine; In tetrahydrofuran; hexane; at -70 - 20℃; for 4.5h; Example 2: Preparation of ethyl 4,4-difluoro-4-chloro-3-oxobutanoic acid (ECDFAA) using a Claissen reaction.n-Butyllithium (85.3 g, 308 mmol) in n-hexane (2.5 M solution) was added dropwise within 30 min to a solution of diisopropylamine (32.7 g, 323 mmol) in THF (200 mL) cooled at -30 to -60 C. The solution was allowed to warm up to 0 C, then cooled down to -70 C and ethyl acetate (26.4 g, 300 mol) was added dropwise during 30 min whilst keeping the temperature at about -60 C.Subsequently, <strong>[383-62-0]ethyl chlorodifluoroacetate</strong> (24.3 g) was added dropwise during 30 min at the same temperature, the mixture was stirred at -65 to -70 C for 3 h, then allowed to warm to room temperature. The mixture was poured onto ice and 4 N HC1 (150 mL) is added. The organic phase was separated and the aqueous phase extracted twice with MTBE. The combined organic phases were washed with 2 N HC1 (100 mL) and saturated sodium chloride solution (100 mL). The organic phase was dried over sodium sulfate, filtered and concentrated under reduced pressure. Ethyl 4-chloro-4,4-difluoro-3-oxo-butanoate (19 g, 61 %) was obtained by distillation (92-94 C; 30 mbar) along with a further mixed fraction. Example 3 : Preparation of ethyl 2-(ethoxymethylene)-4,4-difluoro-3- oxobutanoate (EMEDFAA).A solution of ethyl 4,4-difluoro-3-oxobutanoate (500 g, 3.01 mol), triethyl orthoformate (923 g, 6.23 mmol) and acetic anhydride (784 g, 7.68 mmol) were mixed in a dry glass flask equipped with a small distillation bridge and refluxed at 135 C until no more ethanol is distilled. This procedure was repeated three times; fractionation thus yielded 1575g of EMEDFAA (distillation temperature 106C at 0 mbar) with a yield of 78.5 % and a purity of > 99%.
 

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