METHOD OF SYNTHESIS
    3.
    发明申请
    METHOD OF SYNTHESIS 审中-公开
    合成方法

    公开(公告)号:US20160016874A1

    公开(公告)日:2016-01-21

    申请号:US14773203

    申请日:2013-03-11

    IPC分类号: C07C45/58 C07C45/65 C07C45/76

    摘要: Described is a method of synthesizing 6-(5-ethoxyhept-1-yl)bicyclo[3.3.0] octan-3-one by reacting 3-(5-ethoxyhept-1-yl) cyclopentene with dichloroketene. The resulting reaction products are reacted with acetic acid and zinc to produce 4-(5-ethoxy-hept-1-yl)bicyclo[3.2.0]heptan-6-one and 4-(5-ethoxyhept-1-yl)bicyclo[3.2.0]heptan-7-one, which are reacted with trimethylsulfonium iodide to produce 2-(5-ethoxyhept-1-yl)spiro[bicyclo[3.2.0]heptane-6,2′-oxirane] and 4-(5-ethoxyhept-1-yl)spiro-[bicyclo[3.2.0]heptane-6,2′-oxirane]. Lithium iodide is reacted with 2-(5-ethoxyhept-1-yl)spiro[bicyclo[3.2.0]heptane-6,2′-oxirane] and 4-(5-ethoxyhept-1-yl)spiro-[bicyclo-[3.2.0]heptane-6,2′-oxirane] to produce 6-(5-ethoxyhept-1-yl)bicyclo[3.3.0]octan-3-one. A method of synthesizing 6-(5-methoxyhept-1-yl)bicyclo[3.3.0]octan-3-one is also described.

    摘要翻译: 描述了通过使3-(5-乙氧基庚基-1-基)环戊烯与二氯乙烯酮反应合成6-(5-乙氧基庚-1-基)双环[3.3.0]辛-3-酮的方法。 将所得反应产物与乙酸和锌反应,得到4-(5-乙氧基 - 庚-1-基)双环[3.2.0]庚-6-酮和4-(5-乙氧基庚-1-基)双环 [3.2.0]庚-7-酮,它们与碘化三甲基锍反应生成2-(5-乙氧基庚-1-基)螺[双环[3.2.0]庚烷-6,2'-环氧乙烷]和4- (5-乙氧基庚-1-基)螺 - [双环[3.2.0]庚烷-6,2'-环氧乙烷]。 将碘化锂与2-(5-乙氧基庚-1-基)螺[双环[3.2.0]庚烷-6,2'-环氧乙烷]和4-(5-乙氧基庚-1-基)螺 - [双环 - [3.2.0]庚烷-6,2'-环氧乙烷],得到6-(5-乙氧基庚-1-基)双环[3.3.0]辛-3-酮。 还描述了合成6-(5-甲氧基庚-1-基)双环[3.3.0]辛-3-酮的方法。

    METHOD OF MAKING ALPHA, OMEGA-DIIODOPERFLUOROALKANES
    4.
    发明申请
    METHOD OF MAKING ALPHA, OMEGA-DIIODOPERFLUOROALKANES 有权
    制备ALPHA,OMEGA-DIIODOPERFLUOROKANES的方法

    公开(公告)号:US20150259270A1

    公开(公告)日:2015-09-17

    申请号:US14434981

    申请日:2013-10-09

    IPC分类号: C07C45/58 C07C17/26

    摘要: A method of making α,ω-diiodoperfluoroalkanes includes combining: diatomic iodine, at least one perfluoroalkylene oxide represented by the formula wherein Rf represents a perfluoroalkyl group; and at least one of: a) a first metallic compound comprising nickel, and a second metallic compound comprising molybdenum that is compositionally different from the first metallic compound; or b) a metallic alloy comprising from 50 to 70 percent by weight of nickel and from 20 to 40 percent by weight of molybdenum, based on the total weight of the metallic alloy, thereby producing at least one product represented by the formula I(CF2)nI, wherein n independently represents an integer in the range of from 1 to 11. The total weight of the at least one product wherein n is 3 or greater exceeds the total weight of the at least one product wherein n is 1 or 2 by a factor of at least 4.

    摘要翻译: 制备α,ω-二碘全氟烷烃的方法包括组合:双原子碘,至少一种由下式表示的全氟氧化烯,其中Rf表示全氟烷基; 和至少一种:a)包含镍的第一金属化合物和包含与第一金属化合物成分不同的钼的第二金属化合物; 或b)金属合金,其包含基于金属合金的总重量的50-70重量%的镍和20至40重量%的钼,由此产生至少一种由式I表示的产物(CF 2 )nI,其中n独立地表示1至11范围内的整数。其中n为3或更大的至少一种产物的总重量超过至少一种产物的总重量,其中n为1或2,其中n为1或2, 至少4的因素。

    Reduction of the viscosity of reactive heavy byproducts during the production of 1,3-propanediol
    8.
    发明申请
    Reduction of the viscosity of reactive heavy byproducts during the production of 1,3-propanediol 失效
    在1,3-丙二醇生产过程中降低反应性重副产物的粘度

    公开(公告)号:US20050043570A1

    公开(公告)日:2005-02-24

    申请号:US10676682

    申请日:2003-10-01

    摘要: The present invention is an improvement upon the process for the production of 1,3-propanediol wherein an aqueous solution of 3-hydroxy propanal is formed, catalyst, if any, used in said formation is removed from the solution, sodium hydroxide is added to the solution to neutralize any acid therein such that the pH is at least about 5, the neutralized aqueous solution is subjected to hydrogenation to produce a crude 1,3-propanediol mixture which is distilled to produce 1,3-propanediol, water, and reactive heavy components. The improvement on this process comprises replacing the sodium hydroxide with a hydroxide selected from the group consisting of ammonium hydroxide, alkali metal hydroxides other than sodium hydroxide, and alkaline earth metal hydroxides to reduce the viscosity of the reactive heavy components.

    摘要翻译: 本发明是对生产1,3-丙二醇的方法的改进,其中形成3-羟基丙醛的水溶液,从该溶液中除去所述地层中使用的催化剂(如果有的话),将氢氧化钠加入 中和其中的任何酸使其pH至少约为5的溶液,中和的水溶液进行氢化以产生粗制的1,3-丙二醇混合物,其被蒸馏以产生1,3-丙二醇,水和反应性 重组件。 该方法的改进包括用选自氢氧化铵,氢氧化钠以外的碱金属氢氧化物和碱土金属氢氧化物的氢氧化物代替氢氧化钠,以降低反应性重组分的粘度。

    Purification of 3-hydroxy-propanal
    9.
    发明授权
    Purification of 3-hydroxy-propanal 失效
    纯化3-羟基 - 丙醛

    公开(公告)号:US5986145A

    公开(公告)日:1999-11-16

    申请号:US138314

    申请日:1998-08-21

    摘要: Cobalt or rhodium carbonyl compounds are removed from an aqueous solution of 3-hydroxypropanal by a process comprising the steps of:(a) contacting the 3-hydroxypropanal solution with oxygen under acidic conditions at a temperature within the range of about 5 to about 45.degree. C. to produce an oxidation product mixture comprising an aqueous solution of 3-hydroxypropanal, one or more water-soluble cobalt or rhodium species, and byproduct carbon monoxide;(b) removing byproduct carbon monoxide from the oxidation product mixture as it is generated; and(c) passing the oxidation product mixture in contact with an acidic ion exchange resin maintained at a temperature less than about 45.degree. C. and removing at least a portion of the soluble metal compounds from the oxidation product mixture.Such a process is useful in, for example, the manufacture of 1,3-propanediol from ethylene oxide via an intermediate 3-hydroxypropanal solution containing residual carbon dioxide and insoluble cobalt or rhodium catalyst compounds.

    摘要翻译: 通过包括以下步骤的方法从3-羟基丙醛水溶液中除去羰基钴或铑羰基化合物:(a)在酸性条件下在约5至约45℃的温度范围内使3-羟基丙醛溶液与氧接触 以产生包含3-羟基丙醛水溶液,一种或多种水溶性钴或铑物质和副产物一氧化碳的氧化产物混合物; (b)在生成氧化产物混合物时从副产物一氧化碳中除去; 和(c)使氧化产物混合物与保持在低于约45℃温度的酸性离子交换树脂接触,并从氧化产物混合物中除去至少一部分可溶性金属化合物。 这种方法可用于例如通过含有残余二氧化碳和不溶性钴或铑催化剂化合物的中间体3-羟基丙醛溶液从环氧乙烷制备1,3-丙二醇。

    Method for preparing 3,3-dimethylbutyraldehyde
    10.
    发明授权
    Method for preparing 3,3-dimethylbutyraldehyde 失效
    制备3,3-二甲基丁醛的方法

    公开(公告)号:US5770775A

    公开(公告)日:1998-06-23

    申请号:US796443

    申请日:1997-02-10

    CPC分类号: C07C47/02 C07C45/58

    摘要: A method is disclosed for preparing 3,3-dimethylbutyraldehyde by isomerization of 3,3-dimethylepoxybutane with a basic lithium salt which in turn may be prepared by oxidation of dimethylbutane. The method provides an economical means of preparing 3,3-dimethylbutyraldehyde.

    摘要翻译: 公开了通过用碱性锂盐使3,3-二甲基环氧丁烷异构化制备3,3-二甲基丁醛的方法,碱性锂盐又可以通过二甲基丁烷的氧化来制备。 该方法提供了制备3,3-二甲基丁醛的经济手段。