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    • 5. 发明授权
    • Synthesis of low-fluoride organic compounds
    • 低氟有机化合物的合成
    • US06252105B1
    • 2001-06-26
    • US09348072
    • 1999-07-06
    • Max BraunJohannes EicherFrancine JanssensKerstin EichholzStefan Palsherm
    • Max BraunJohannes EicherFrancine JanssensKerstin EichholzStefan Palsherm
    • C07C6963
    • C07C67/56C07C51/47C07C51/64C07C53/18C07C67/14C07C67/58C07C53/48C07C59/195C07C69/63C07C69/72
    • Organic compounds, e.g. fluorinated organic compounds such as fluorinated carboxylic acids or fluorinated carboxylic acid chlorides, may contain small amounts of carboxylic acid fluorides, hydrogen fluoride or hydrolyzable fluoride, which during the preparation of derivatives of the fluorinated organic compounds, for example by esterification, may yield corrosive fluorides or hydrogen fluoride. The invention is a method for the synthesis and/or purification of preferably fluorinated organic compounds such as carboxylic acids, carboxylic acid chlorides and derivatives such as esters thereof, starting from corresponding carboxylic acid chlorides containing acid fluorides or hydrolyzable fluoride, and alcohols under the catalytic action of “onium” salts of carboxylic acids, to obtain products which have a low fluoride content. Alternatively, an inorganic oxide adsorbent is utilized. The method is especially suitable for the synthesis of esters of trifluoroacetic acid, chlorodifluoroacetic acid, trifluoroacetoacetic acid and/or difluoroacetoacetic acid.
    • 有机化合物,例如 含氟有机化合物如氟化羧酸或氟化羧酸氯化物可含有少量羧酸氟化物,氟化氢或水解性氟化物,其在氟化有机化合物衍生物的制备过程中,例如通过酯化反应,可产生腐蚀性氟化物 或氟化氢。 本发明是一种合成和/或纯化优选氟化有机化合物如羧酸,羧酸氯化物及其衍生物如酯的方法,起始于含有酸性氟化物或可水解氟化物的相应的羧酸氯化物和催化剂下的醇 羧酸的“鎓”盐的作用,以获得具有低氟含量的产物。 或者,使用无机氧化物吸附剂。 该方法特别适用于三氟乙酸,氯二氟乙酸,三氟乙酰乙酸和/或二氟乙酰乙酸的酯的合成。
    • 10. 发明授权
    • Process for chemical synthesis from an alkenone made from a halogenated precursor
    • 由卤化前体制成的烯酮进行化学合成的方法
    • US08957254B2
    • 2015-02-17
    • US14046171
    • 2013-10-04
    • Max BraunStefan PalshermUta ClaassenAlain Lambert
    • Max BraunStefan PalshermUta ClaassenAlain Lambert
    • C07C45/41C07D211/02C07D213/64C07D401/00C07C45/65
    • C07C45/41C07C45/65C07C49/175C07C49/255
    • Process for synthesizing a chemical, in particular an agriculturally or pharmaceutically active compound, including: a first step comprising reacting a carboxylic acid halide with a vinyl ether to prepare a halogenated precursor of an alkenone; a second step comprising eliminating hydrogen halide from such precursor to form an alkenone, preferably by thermolysis under specific conditions; and a third step which uses the formed alkenone as a building block to synthesize the chemical. First step may be done in a liquid reaction medium comprising an alkenone or a halogenated alkenone precursor, or in a liquid reaction medium in turbulent state, specifically by creation of gas bubbles of the carboxylic acid halide herein. Second step may include a flash thermolysis, vacuum thermolysis, thermolysis under stripping with inert gas, and/or a thermolysis at a temperature from >90° C. to 120° C. Third step preferably comprises reacting the alkenone with a nitrogen-containing compound.
    • 用于合成化学品,特别是农业或药学活性化合物的方法,包括:第一步,包括使羧酸卤化物与乙烯基醚反应以制备烯酮的卤化前体; 第二步,包括从这种前体消除卤化氢以形成烯酮,优选通过在特定条件下的热解; 和使用形成的烯酮作为结构单元合成化学品的第三步骤。 第一步可以在包含烯酮或卤代烯酮前体的液体反应介质中或在湍流状态的液体反应介质中,特别是通过产生本文中的羧酸卤化物的气泡进行。 第二步骤可以包括闪蒸热解,真空热解,用惰性气体汽提时的热解,和/或在> 90℃至120℃的温度下的热解。第三步优选包括使烯酮与含氮化合物 。