| 摘要 |
New method for working up mixtures obtained by chlorine/fluorine exchange reactions with alkali metal fluoride in presence of quaternary ammonium or phosphonium compounds, ethers or crown ethers involves adding water, mixing vigorously and separating off the aqueous phase. A method for working up reaction mixtures containing compounds of formula (I). AZxArFwCl(y-w)Rz (I) Az = F, Cl, Br, NO2, CN, CF3, CCl3, CHO, -CO(1-10C alkyl), -COX or -SO2X; X = F, Cl or Br; x = 1-3; Ar = phenyl, pyridyl or naphthyl; w = 1-y; y = 1-5; R = H, or optionally branched 1-10C alkyl or alkoxy; z = 1-5; (x + y + z) = total substitutable valencies on Ar, which are obtained by reacting compounds of formula AzxArClyRz (II) with alkali metal fluoride(s) at 50-250 degrees C in presence of a component (a) or a mixture of (a) and at least one of the components (b), (c), (d) and (e) as catalyst and in presence or absence of solvent. The process involves adding water to the mixture containing (I), bringing the components into intimate contact and separating off the aqueous phase. Components (a)-(e) comprise quaternary ammonium compounds, amidophosphonium salts, quaternary phosphonium compounds, ethers and crown ethers of formula (III), (IV), (V), (VI) and (VII) respectively, R<1>-R<3> = optionally branched groups of formula -(CmH2mO)pR<5>, 1-30C alkyl, or phenyl or naphthyl (optionally substituted with halogen, 1-4C alkyl or alkoxy, nitro or cyano); R<4> = -(CmH2mO)pR<5> as above; X = a mono- or multi-valent acid residue; A<1>-A<8> = 1-12C alkyl or alkenyl, 4-8C cycloalkyl, 6-12C aryl or 7-12C aralkyl, or A<1>A<2>, A<3>A<4>, A<5>A<6> and A<7>A<8> may combine to form 3- to 7-membered rings (optionally with O or NR<9> in the ring); A<9> = 1-4C alkyl; R<6>-R<9> = 1-22C alkyl, aryl or (1-4C alkyl)-aryl, with aryl = phenyl or naphthyl (optionally substituted as above); R<10>, R<11> = 1-16C alkyl; a = 2-6; and b = 0-20.
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