Reaktion #526850

ord-d22647f8097840ec8bd3c2498b37f21a

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Vorschrift

In the second method the synthesis of 4-bromo-3-chloro-3,4,4-trifluorobutanoic acid (VIII) is followed by zinc dehalogenation to produce 3,4,4-trifluoro-3-butenoic acid (IV). This compound is prepared by reacting 1-chloro-1,2-dibromotrifluoroethane (VI) with ethyl vinyl ether in the presence of sodium dithionite and sodium bicarbonate in a manner analogous to that described in the literature Huang, Weiyuan; Lu, Long;, Zhang, Yuanfa; Chin. J. Chem. 1990, (3), 281!. However, it is now found that the 4-bromo-3-chloro-3,4,4-trifluorobutanal intermediate (VII) is oxidized without isolation with sodium chlorite/hydrogen peroxide. In other words, instead of oxidation with Jones reagent, this method advantageously provides a process which can be carried out in one reaction vessel using preferred reagents and gives an unexpectedly high yield.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05514717uspto-grants-1996_05