Preparation of O,S-dimethyl-thiolophosphoric acid amide
    1.
    发明授权
    Preparation of O,S-dimethyl-thiolophosphoric acid amide 失效
    制备O,S-二甲基 - 硫代磷酸酰胺

    公开(公告)号:US4537730A

    公开(公告)日:1985-08-27

    申请号:US516167

    申请日:1983-07-21

    IPC分类号: C07F9/24

    CPC分类号: C07F9/24

    摘要: A simplified process for preparing the known insecticide 0,S-dimethylthiolphosphoric acid amide of the formula ##STR1## inexpensively, in high purity and with minimum waste water and gas which would have to be specially treated to avoid environmental pollution, comprises(a) contacting 0,0 dimethyl-thiophosphoric acid amide of the formula ##STR2## in which Me is sodium or potassium, separating the aqueous phase,(b) optionally adding an organic solvent to the aqueous phase, and reacting the mass with methyl bromide or methyl chloride thereby to form the 0,S-dimethyl-thiolphosphoric acid amide, and either(c) extracting the amide with a sparingly water-miscible solvent thereby to dissolve the amide, or(d) concentrating the reaction mixture from the methylation step (b), by distillation, until the alkali metal halide formed has separated out, and filtering off the alkali metal halide.

    摘要翻译: 制备低成本的已知杀虫剂0,S-二甲基硫代磷酸酰胺的简便方法是以高纯度和最少的废水和气体制备,该方法必须经过特殊处理以避免环境污染,其包括(a)接触 其中Me是钠或钾的0,0二甲基 - 硫代磷酸酰胺,其中Me是钠或钾,分离水相,(b)任选地向水相中加入有机溶剂,并使该物质与甲基溴或甲基氯 从而形成0S-二甲基 - 硫醇磷酸酰胺,和(c)用少量与水混溶的溶剂萃取酰胺,从而溶解酰胺,或(d)从甲基化步骤(b)浓缩反应混合物, 通过蒸馏,直到形成的碱金属卤化物分离出来,并过滤掉碱金属卤化物。

    Process for preparing O-alkyl, O-alkylphosphorochloridothioates
    2.
    发明授权
    Process for preparing O-alkyl, O-alkylphosphorochloridothioates 失效
    O-烷基,O-烷基磷酰氯化物的制备方法

    公开(公告)号:US5948930A

    公开(公告)日:1999-09-07

    申请号:US927850

    申请日:1997-09-11

    IPC分类号: C07F9/20 C07F9/16

    CPC分类号: C07F9/20

    摘要: The invention relates to process for the preparation of an O-alkyl, O-alkyl phosphorochloridothioate by 1) reacting A) a thiophosphoryl halide with B) an alcohol, in the presence of C) a tertiary amine acid acceptor and D) a solvent, and 2) reacting the resultant product with a second alcohol, different from the alcohol used in step 1). In the preferred embodiment, the intermediate product is not isolated before reaction with the second alcohol.

    摘要翻译: 本发明涉及通过以下步骤制备O-烷基,O-烷基氯代硫代磷酸酯的方法:1)在C)叔胺酸受体和D)溶剂的存在下,使A)硫代磷酰卤与B)醇反应, 和2)使所得产物与不同于步骤1)中使用的醇的第二醇反应。 在优选的实施方案中,中间产物在与第二醇反应之前不分离。

    Preparation of .epsilon.-caprolactone
    3.
    发明授权
    Preparation of .epsilon.-caprolactone 失效
    ε-己内酯的制备

    公开(公告)号:US4341709A

    公开(公告)日:1982-07-27

    申请号:US150260

    申请日:1980-05-15

    CPC分类号: C07D315/00

    摘要: A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.

    摘要翻译: 一种制备ε-己内酯的方法,包括:(a)使环己酮与过丙酸在有机溶剂中的溶液以环己酮的摩尔比约1.1-5:1的约0.1〜5:1的摩尔比在约10℃〜 形成基本上由ε-己内酯,丙酸和有机溶剂组成的反应混合物,(b)在第一蒸馏单元中将反应混合物从(a)中蒸馏,得到包含有机溶剂和蒸馏残余物的馏出物 (c)在一点将来自(b)的蒸馏残余物引入第二蒸馏单元以获得包含丙酸和未反应的环己酮的馏出物,从第二蒸馏单元彼此分离并在低于 引入第二蒸馏装置,ε-己内酯和任何高沸点组分,和(d)在第三蒸馏装置中蒸馏出馏出物(c)得到 基本上由丙酸组成的馏出物和包含丙酸和环己酮的混合物的蒸馏残渣。

    Process for preparing heterocyclic compounds
    5.
    发明授权
    Process for preparing heterocyclic compounds 有权
    制备杂环化合物的方法

    公开(公告)号:US06211379B1

    公开(公告)日:2001-04-03

    申请号:US09488436

    申请日:2000-01-20

    IPC分类号: C07D41706

    CPC分类号: C07D417/06

    摘要: The present application relates to a process for preparing compounds of the formula (I) in which R1, A, X and Z are each as defined in the description by reacting compounds of the formula (II) in which A and X are each as defined in the description with compounds of the formula (III) in which Z, R1 and M1 are each as defined in the description.

    摘要翻译: 本申请涉及一种制备式(I)化合物的方法,其中R 1,A,X和Z各自如说明书中所定义,通过使式(II)化合物(其中A和X各自如上所定义) 在其中Z,R 1和M 1各自如说明书中所定义的式(III)化合物的描述中。

    Process for the preparation of propylene oxide
    7.
    发明授权
    Process for the preparation of propylene oxide 失效
    环氧丙烷的制备方法

    公开(公告)号:US4113747A

    公开(公告)日:1978-09-12

    申请号:US678822

    申请日:1976-04-28

    IPC分类号: C07C409/24 C07D301/14

    摘要: Process for continuous production of propylene oxide (FIG. 1) from propylene and aqueous hydrogen peroxide. The aqueous hydrogen peroxide is first reacted with propionic acid in the presence of acid catalyst to form perpropionic acid (1). The perpropionic acid is taken up by extraction in benzene (5 , 12), and following drying of the benzene solution (16), the perpropionic acid in the solution is reacted with propylene (18) for oxidation of the propylene to propylene oxide and conversion of the perpropionic acid back to propionic acid. The reaction mixture is worked up to separate propylene oxide, propionic acid and benzene (25, 27, 31, 33), and the latter two are recycled. In the benzene extraction (5, 12), an aqueous raffinate (7) is formed containing hydrogen peroxide and acid catalyst. Water is removed from the aqueous raffinate (8) and the concentrate is recycled to the propionic acid reactor. Make-up hydrogen peroxide can be added to the aqueous raffinate before the removal of water.

    摘要翻译: 从丙烯和过氧化氢水溶液连续生产环氧丙烷(图1)的方法。 过氧化氢水溶液首先在酸催化剂存在下与丙酸反应形成过丙酸(1)。 通过在苯(5,12)中萃取,过丙酸被吸收,然后在苯溶液(16)干燥后,将溶液中的过丙酸与丙烯(18)反应,将丙烯氧化成环氧丙烷并转化 的过丙酸回到丙酸。 处理反应混合物以分离环氧丙烷,丙酸和苯(25,27,31,33),后两者被再循环。 在苯提取(5,12)中,形成含有过氧化氢和酸催化剂的残液水溶液(7)。 水从残液(8)中除去,浓缩物再循环到丙酸反应器中。 在除去水之前,可以将补充过氧化氢加入含水残液中。