Manufacturing method for phosphonic acid derivatives
    1.
    发明授权
    Manufacturing method for phosphonic acid derivatives 失效
    膦酸衍生物的制备方法

    公开(公告)号:US5679844A

    公开(公告)日:1997-10-21

    申请号:US605056

    申请日:1996-03-01

    IPC分类号: C07F9/38

    CPC分类号: C07F9/3813

    摘要: The present invention relates to a method of manufacturing N-phosphonomethylglycine and salts thereof, which can be biologically degraded, and have superior effectiveness against weeds and are useful as herbicides, by means of alkali hydrolysis of N-phosphonomethylglycinonitrile. In order to obtain high yields of the desired high purity, the amount of salt produced as a by-product is reduced by using the alkali so as to result in not less than 2 molecules and less than 3 molecules of the alkali for each molecule of N-phosphonomethylglycinonitrile when the alkali is monovalent, and not less than 1 molecule and less than 1.5 molecules of the alkali for each molecule of N-phosphonomethylglycinonitrile when the alkali is divalent.

    摘要翻译: PCT No.PCT / JP95 / 01327 Sec。 371日期1996年3月1日 102(e)1996年3月1日PCT PCT 1995年7月3日PCT公布。 出版物WO96 / 01264 日期1996年1月18日本发明涉及N-膦酰基甲基甘氨酸及其盐的制造方法,其可以生物降解,并且对于杂草具有优异的有效性,并且通过N-膦酰基甲基甘氨腈的碱水解可用作除草剂。 为了获得所需高纯度的高产率,通过使用碱来降低作为副产物产生的盐的量,从而得到每个分子的不少于2个分子和少于3个碱的分子 当碱为二价时,N-膦酰基甲基甘氨腈为N-膦酰基甲基甘氨腈,当碱为二价时,每分子N-膦酰基甲基甘氨腈为1分子以上且小于1.5分子的碱。

    Method for isolating N-phosphonomethylglycine
    3.
    发明授权
    Method for isolating N-phosphonomethylglycine 失效
    N-膦酰基甲基甘氨酸的分离方法

    公开(公告)号:US5859289A

    公开(公告)日:1999-01-12

    申请号:US814830

    申请日:1997-03-11

    IPC分类号: A01N57/20 C07F9/38

    CPC分类号: A01N57/20 C07F9/3813

    摘要: The present invention provides a method for isolating N-phosphonomethylglycine which comprises adding an acid to precipitate salts from an aqueous solution of an alkali metal salt and/or an alkaline earth metal salt of N-phosphonomethylglycine solution to neutralize and adjust the same to a pH of 2.5 or higher, removing the precipitated salts, and adjusting the pH to 2.5 or lower to crystallize N-phosphonomethylglycine. N-phosphonomethylglycine is thus isolated and purified in high purity and good yield.

    摘要翻译: 本发明提供了一种分离N-膦酰基甲基甘氨酸的方法,该方法包括加入酸以从N-膦酰基甲基甘氨酸溶液的碱金属盐和/或碱土金属盐的水溶液中沉淀出盐,以将其调节至pH 2.5或更高,去除沉淀的盐,并将pH调节至2.5以下以结晶N-膦酰基甲基甘氨酸。 因此N-膦酰基甲基甘氨酸以高纯度和良好的产率分离和纯化。

    Method for producing N-phosphonomethylglycine
    4.
    发明授权
    Method for producing N-phosphonomethylglycine 失效
    N-膦酰基甲基甘氨酸的制备方法

    公开(公告)号:US5750774A

    公开(公告)日:1998-05-12

    申请号:US814827

    申请日:1997-03-11

    IPC分类号: C07F9/38

    CPC分类号: C07F9/3813

    摘要: The present invention provides a method for producing N-phosphonomethylglycine which comprises reacting an aminomethylphosphonic acid with glycolonitrile, or formaldehyde and hydrogen cyanide in situ, under an alkaline condition to convert the aminomethylphosphonic acid into an N-phosphonomethylglycinonitrile salt or a mixture of an N-phosphonomethylglycinonitrile salt and N-phosphonomethylglycinonitrile, and then hydrolyzing the product under an acidic condition. Subsequent to a reaction step for the production of N-phosphonomethylglycinonitrile, the reaction product is hydrolyzed by adding thereto an acid in a prescribed amount. Accordingly, the use of a large amount of an alkaline metal hydroxide and the neutralization step for obtaining N-phosphonomethylglycine after hydrolysis, which steps are necessary in a conventional alkali hydrolysis method, are omitted in the present invention.

    摘要翻译: 本发明提供了一种N-膦酰基甲基甘氨酸的制备方法,该方法包括使氨基甲基膦酸与乙醇腈或甲醛和氰化氢在碱性条件下原位反应,将氨基甲基膦酸转化为N-膦酰基甲基甘氨腈盐或N- 膦酰基甲基甘氨腈盐和N-膦酰基甲基甘氨腈,然后在酸性条件下水解产物。 在制备N-膦酰基甲基甘氨腈的反应步骤之后,通过向其中加入规定量的酸来水解反应产物。 因此,在本发明中,省略了大量碱金属氢氧化物的使用和水解后得到N-膦酰基甲基甘氨酸的中和工序,这些步骤在常规碱水解法中是必需的。

    Preparation of N-acylaminomethylphosphonic acid
    5.
    发明授权
    Preparation of N-acylaminomethylphosphonic acid 失效
    N-酰氨基甲基膦酸的制备

    公开(公告)号:US5324855A

    公开(公告)日:1994-06-28

    申请号:US961363

    申请日:1992-10-15

    IPC分类号: C07F9/24 C07F9/38

    CPC分类号: C07F9/3813

    摘要: N-acylaminomethylphosphonic acid is prepared from an N-methylolamide compound and a phosphorus trihalide. The starting compounds are mixed and heated in an aprotic solvent in the presence of water in a 0.25 to 2.5 times molar amount relative to the phosphorus trihalide at 60.degree. to 160.degree. C., and the reaction mixture is contacted with water. The N-methylolamide compound is a compound selected from the group consisting of N-methylol-lower alkylamides and N-methylolarylamides. The phosphorus trihalide is preferably phosphorus trichloride. As the aprotic solvent is used one or more of hydrocarbons, halogenated hydrocarbons, ethers, polyethers, nitriles, and aromatic nitro compounds. The mixing may be carried out at a temperature of 60.degree. C. The water present at the initiation of the reaction is in a 1.0 to 1.8 times molar amount relative to the phosphorus trihalide.

    摘要翻译: N-酰氨基甲基膦酸由N-羟甲基酰胺化合物和三卤化磷制备。 将起始化合物在非质子溶剂中在相对于三卤化磷在0.25至160℃下以0.25至2.5倍摩尔量存在的水中加热,并将反应混合物与水接触。 N-羟甲基酰胺化合物是选自N-羟甲基 - 低级烷基酰胺和N-羟甲基芳基酰胺的化合物。 三卤化磷优选为三氯化磷。 由于非质子溶剂使用一种或多种烃,卤代烃,醚,聚醚,腈和芳族硝基化合物。 混合可以在60℃的温度下进行。反应开始时存在的水相对于三卤化磷的摩尔量为1.0〜1.8倍。

    Non-hygroscopic crystals of p-aminomethylbenzoic acid and process for
preparing the same
    7.
    发明授权
    Non-hygroscopic crystals of p-aminomethylbenzoic acid and process for preparing the same 失效
    对氨基甲基苯甲酸的非吸湿性晶体及其制备方法

    公开(公告)号:US5777158A

    公开(公告)日:1998-07-07

    申请号:US917688

    申请日:1997-08-26

    CPC分类号: C07C227/42 C07C229/38

    摘要: The novel non-hygroscopic crystals of p-aminomethylbenzoic acid can be obtained by heating hygroscopic crystals of p-aminomethylbenzoic acid with keeping the hygroscopic crystals in contact with moisture to transit the hygroscopic crystals to non-hygroscopic crystals. The non-hygroscopic crystals of p-aminomethylbenzoic acid can be particularly advantageously handled in the atmosphere as compared with the conventional hygroscopic crystals. Especially when the p-aminomethylbenzoic acid is used for the non-aqueous reaction, the crystals of the invention are exceptionally advantageous from the viewpoints of removal of moisture and humidity control.

    摘要翻译: 对氨基甲基苯甲酸的新型非吸湿性结晶可以通过加热对氨基甲基苯甲酸的吸湿结晶,同时保持吸湿结晶与水分接触,使吸湿性晶体转移到非吸湿性晶体。 与常规吸湿晶体相比,对氨基甲基苯甲酸的非吸湿性结晶可以特别有利地在大气中处理。 特别是当对氨基甲基苯甲酸用于非水反应时,从除去湿气和湿度控制的观点来看,本发明的结晶是非常有利的。

    Method for manufacturing 3-isochromanone
    9.
    发明授权
    Method for manufacturing 3-isochromanone 失效
    3-异色满酮的制备方法

    公开(公告)号:US06180801B2

    公开(公告)日:2001-01-30

    申请号:US09277941

    申请日:1999-03-29

    IPC分类号: C07D31102

    CPC分类号: C07D311/76

    摘要: The present invention intends to provide a method for producing 3-isochromanones represented by formula (II) useful as a synthetic starting material of medicals or agricultural chemicals and the cyano compound represented by formula (I) by an industrially advantageous method in a high yield. Disclosed herein is a method for manufacturing a 3-isochromanone represented by the following formula (II): (wherein R2, R3, R4 and R5 each independently represents a hydrogen atom, a halogen atom, an alkyl group or an alkoxy group), said method is characterized by comprising the steps of: hydrolyzing a cyano compound represented by formula (I): (wherein R1 represents a hydrogen atom, an alkyl group or an aryl group, and R2, R3, R4 and R5 have the same meanings as defined above) and subjecting the hydrolyzate to intra-molecular cyclization.

    摘要翻译: 本发明意在提供一种由工业上有利的方法以高产率制备可用作医药或农药合成原料的式(II)表示的3-异色满酮和由式(I)表示的氰基化合物的方法。 本文公开了一种制备由下式(II)表示的3-异色满酮的方法:其中R2,R3,R4和R5各自独立地表示氢原子,卤原子,烷基或烷氧基),所述 方法的特征在于包括以下步骤:水解由式(I)表示的氰基化合物:(其中R1表示氢原子,烷基或芳基,R2,R3,R4和R5具有与定义相同的含义) 并使水解产物进行分子内环化。