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    • 6. 发明申请
    • FLUORINATED ALKYLTHIOCYANATE PROCESS
    • 氟化烷基铝酸盐工艺
    • WO1998025894A1
    • 1998-06-18
    • PCT/US1997022582
    • 1997-12-10
    • E.I. DU PONT DE NEMOURS AND COMPANY
    • E.I. DU PONT DE NEMOURS AND COMPANYJACOBSON, Stephen, Ernest
    • C07C331/04
    • C07C331/10C07C331/04C07C331/12C07C331/14
    • A process for the preparation of a thiocyanate of the Formula (II): Rf-Am-(CH2)n-SCN wherein Rf is a C2-C20 perfluoroalkyl radical, or a C5-C38 perfluoroalkyl radical having at least one ether oxygen atom; n is 1 to 3; m is 0 or 1; A is O, S, CO2, N(R1)R2, CON(R1)R2, SO2N(R1)R2 or (OCH2CHR3)aO; wherein a is 3 to about 15; R1 is H or alkyl radical of 1 to about 4 carbon atoms; R2 is C1-C12alkylene; and R3 is H or CH2Cl; said process comprising reacting a fluorinated iodide of the Formula (I): Rf-Am-(CH2)n-I wherein Rf, A, m and n are as defined above, with a thiocyanate salt M (SCN) wherein M is sodium or potassium, in the presence of a catalyst comprising a quaternary ammonium salt of the Formula (R4)3(R5)N Y wherein R4 is butyl; R5 is methyl or butyl; and Y is Cl, Br, I, or HSO4; to yield the fluorinated thiocyanate of Formula (II) as defined above is disclosed.
    • 制备式(II)的硫氰酸酯的方法:Rf-Am-(CH2)n-SCN,其中Rf是C2-C20全氟烷基或具有至少一个醚氧原子的C5-C38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) 其中a为3至约15; R1是H或1至约4个碳原子的烷基; R2是C1-C12亚烷基; 并且R 3是H或CH 2 Cl; 所述方法包括使式(I)的氟化碘:Rf-Am-(CH 2)n I,其中Rf,A,m和n如上定义,与硫氰酸盐M +(SCN) - 在含有式(R4)3(R5)N + Y的季铵盐的催化剂存在下,M是钠或钾,其中R 4是丁基; R5是甲基或丁基; Y是Cl,Br,I或HSO4; 得到如上定义的式(II)的氟化硫氰酸酯。