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    • 1. 发明申请
    • METHOD OF SYNTHESIZING TETRAFLUOROPHTHALONITRILE
    • 合成四氢呋喃酮的方法
    • WO1987007267A1
    • 1987-12-03
    • PCT/US1986002662
    • 1986-12-10
    • ALLIED CORPORATION
    • ALLIED CORPORATIONNALEWAJEK, DavidLOCKYER, George, DonaldEIBECK, Richard, ElmerPYSZCZEK, Michael, Francis
    • C07C121/50
    • C07C255/00C07C51/08C07C51/363C07C63/68
    • A process for the preparation of compounds of the general formula C6Fx(CN)y, wherein x and y are whole integers whose sum equals 6. The process is particularly useful for the synthesis of fluorinated nitriled containing at least two cyano groups (y=2). Among the preferred compounds prepared is tetrafluorophthalonitrile, a key intermediate used as a building block in the pharmaceutical industry. In the process described, tetrafluorophthalonitrile is prepared by the reaction of a chlorinated compound of general formula C6Clx(CN)y wherein x and y are whole integers whose sum equals 6. Specifically, tetrachlorophthalonitrile is reacted with potassium fluoride in an aprotic solvent to prepare tetrafluorophthalonitrile. The fluoronitrile is produced in at least 80 % yield and a minimum purity of 98.5 %. Only one additional recrystallization is required to produce a material of > 99.5 % purity. In another embodiment, the crude tetrafluorophthalonitrile is recrystallized from a hydrocarbon alkane solvent to produce a product of > 99.5 % purity which can be used directly as an intermediate. This process represents an economical means to produce tetrafluorophthalonitrile on an industrial scale.
    • 制备通式为C 6 F x(CN)y的化合物的方法,其中x和y是总和等于6的整数。该方法特别可用于合成含有至少两个氰基的氟化腈(y = 2 )。 在制备的优选化合物中,四氟邻苯二甲腈是制药工业中用作结构单元的关键中间体。 在所述方法中,四氟邻苯二腈通过与通式C 6 Cl x(CN)y的氯化化合物反应制备,其中x和y为总和为6的整数。具体地说,四氟邻苯二腈与氟化钾在非质子传递溶剂中反应制备四氟邻苯二甲腈 。 氟代腈的产率至少为80%,最低纯度为98.5%。 需要再进行一次再结晶以制备纯度> 99.5%的材料。 在另一个实施方案中,将粗四氟邻苯二甲腈从烃烷烃溶剂中重结晶以产生可直接用作中间体的> 99.5%纯度的产物。 该方法代表在工业规模上生产四氟邻苯二腈的经济手段。