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    • 8. 发明授权
    • Fluorinated alkylthiocyanate process
    • 氟化烷基硫氰酸酯工艺
    • US5726337A
    • 1998-03-10
    • US766717
    • 1996-12-13
    • Stephen Ernest Jacobson
    • Stephen Ernest Jacobson
    • B01J31/02C07B61/00C07C331/04C07C331/10C07C331/12C07C331/14C07C331/02
    • C07C331/10C07C331/04C07C331/12C07C331/14
    • A process for the preparation of a thiocyanate of Formula II R.sub.f --A.sub.m --(CH.sub.2).sub.n --SCN II wherein R.sub.f is a C.sub.2 -C.sub.20 perfluoroalkyl radical, or a C.sub.5 -C.sub.38 perfluoroalkyl radical having at least one ether oxygen atom; n is 1 to 3; m is 0 or 1; A is O, S, CO.sub.2, N(R.sub.1)R.sub.2, CON(R.sub.1)R.sub.2, SO.sub.2 N(R.sub.1 R.sub.2 or (OCH.sub.2 CHR.sub.3).sub.a O; wherein a is 3 to about 15; R.sub.1 is H or alkyl radical of 1 to about 4 carbon atoms; R.sub.2 is C.sub.1 -C.sub.12 alkylene; and R.sub.3 is H or CH.sub.2 Cl; said process comprising reacting a fluorinated iodide of Formula I R.sub.f --A.sub.m --(CH.sub.2).sub.n --I I wherein R.sub.f, A, m and n are as defined above, with a thiocyanate salt M.sup.+ (SCN).sup.- wherein M is sodium or potassium, in the presence of a catalyst comprising a quaternary ammonium salt of formula (R.sub.4).sub.3 (R.sub.5)N.sup.+ Y.sup.- wherein R.sub.4 is butyl; R.sub.5 is methyl or butyl; and Y is Cl, Br, I, or HSO.sub.4 ; to yield the fluorinated thiocyanate of Formula II as defined above is disclosed.
    • 制备式II的硫氰酸盐的方法Rf-Am-(CH 2)n-SCN II,其中R f是C 2 -C 20全氟烷基或具有至少一个醚氧原子的C 5 -C 38全氟烷基; n为1〜3; m为0或1; A是O,S,CO 2,N(R 1)R 2,CON(R 1)R 2,SO 2 N(R 1 R 2或(OCH 2 CHR 3))a;其中a为3至约15; R 1为H或1至约4个碳原子的烷基 ; R 2是C 1 -C 12亚烷基; R 3是H或CH 2 Cl;所述方法包括使式I的Rf-Am-(CH 2)n-II的氟化碘化物,其中Rf,A,m和n如上定义,与硫氰酸酯 盐M +(SCN) - 其中M是钠或钾,在包含式(R4)3(R5)N + Y-的季铵盐的催化剂存在下,其中R 4是丁基; R 5是甲基或丁基; Y 是Cl,Br,I或HSO 4;得到如上定义的式II的氟化硫氰酸酯。