1583-59-1

Hazard Information

Chemical Properties

Colorless to pale yellow liquid

Synthesis

274-09-9

1583-59-1

The general procedure for synthesizing 2,2-difluoro-1,3-benzodioxole from piperylene ring was as follows: first, 100 g of benzodioxole and 900 g of acetonitrile were accurately weighed and mixed to prepare a solution of benzodioxole acetonitrile with a mass fraction of 10%. Subsequently, 1 g of trifluoroacetic acid was added to this solution and mixed thoroughly. Next, a fluorine gas-nitrogen mixture with a mass fraction of 10% was prepared by adjusting the flow rate of fluorine gas and nitrogen gas. The reaction process shown in FIG. 1 was employed, using a microchannel reactor made of silicon carbide. The liquid volume of each module was set to 1 ml and the reaction temperature was controlled at -20 °C. The reaction residence time was controlled by adjusting the pumping rate to 20 s. In module A, a 10% mass fraction benzodioxole acetonitrile solution containing 1% trifluoroacetic acid was continuously pumped for pre-cooling. At the same time, a 10% mass fraction fluorine gas mixture was continuously and uniformly passed into the B module, in which the molar amount of fluorine gas was 2.2 times that of benzodioxole. After the reactants were mixed and reacted in the CDEF module, they entered a gas-liquid separator for separation. The separated gas was treated and discharged, while the liquid was washed and distilled, resulting in 1,3-benzodioxole-2,2-difluorine product with 90% yield and 99% content.

Questions And Answer

• Uses

  2,2-Difluoro-1,3-benzodioxole is an intermediate compound which is used especially for the preparation of products for agricultural chemistry and for the synthesis of pharmaceutical products.
  2,2-difluoro-1,3-benzodioxole is a useful difluoromethylated building block for the synthesis of various benzodioxole-containing pharmaceutical active compounds.
  2-,3-,and 4-(Trifluoromethoxy)phenyllithiums: Versatile intermediates offering access to a variety of new organofluorine compounds.
  Selective aliphatic fluorination by halogen exchange in mild conditions. ;

• Preparation

  2,2-Difluoro-1,3-benzodioxole is prepared by reaction of 2,2-dichloro-1,3-benzodioxole with potassium fluoride in the presence of an effective quantity of a catalyst selected from potassium hydrogen fluoride, sodium hydrogen fluoride, cesium hydrogen fluoride, rubidium hydrogen fluoride, and quaternary ammonium hydrogen fluoride.
  https://patents.google.com/patent/US5432290A/en ;

• References

  [1] E.Castagnetti, et al, Eur. J. Org. Chem., 2001, 2001(4), pp 691-695.
  [2] L.Saint-Jalmes, J. F. Chem., 2006, 127(1), pp 85-90. ;

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