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    • 4. 发明申请
    • Process for the preparation of $g(e)-caprolactam
    • 制备$ g(e) - 己内酰胺的方法
    • US20040132999A1
    • 2004-07-08
    • US10473077
    • 2004-02-27
    • Wim BuijsHenricus Franciscus Wilhelmus
    • C07D201/02
    • C08G69/16C07D201/08
    • The invention relates to a process for the preparation of null-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation using superheated steam characterized in that the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam. The invention also relates to a process for the preparation of null-caprolactam starting from 6-aminocapronitrile by hydrolysis/oligomerisation followed by de-oligomerisation/cyclisation characterized in that the preparation is performed in a horizontal scraped-surface reactor, the hydrolysis/oligomerisation is performed with superheated steam converting 6-aminocapronitrile into a molten phase and a gas phase comprising ammonia, ammonia is continuously separated off and the de-oligomerisation/cyclisation is performed by treating the molten phase further with superheated steam.
    • 本发明涉及一种从6-氨基己腈开始通过水解/低聚制备ε-己内酰胺的方法,然后使用过热蒸汽进行脱低聚/环化,其特征在于水解/低聚反应用过热蒸汽将6-氨基己腈转化成 熔融相和包含氨的气相,氨被连续分离,并且通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。 本发明还涉及从6-氨基己腈开始制备ε-己内酰胺的方法,其通过水解/低聚,接着进行脱低聚/环化,其特征在于制备在水平刮面反应器中进行,水解/低聚是 使用过热蒸汽将6-氨基己腈转化成熔融相和包含氨的气相,连续分离氨,通过用过热蒸汽进一步处理熔融相进行脱低聚/环化。
    • 5. 发明申请
    • Method for the production of caprolactam
    • 生产己内酰胺的方法
    • US20030153749A1
    • 2003-08-14
    • US10297209
    • 2002-12-04
    • Frank OhlbachAndreas AnsmannRolf-Hartmuth FischerJohann-Peter Melder
    • C07D201/02
    • C07D201/08Y02P20/52
    • A process is provided for the preparation of caprolactam from a compound of formula (I): NCnull(CH2)5nullCOnullRnullnull(I)in which R is a carboxamide, carboxylic acid or carboxylic acid ester group, wherein a) a compound (I) or a mixture of such compounds, in the presence of ammonia and optionally a liquid diluent (VI), is hydrogenated with hydrogen in the presence of a catalyst (II) to give a mixture (III), b) the hydrogen and the catalyst (II) are separated from the mixture (III) to give a mixture (IV), and c) the mixture (IV), optionally in the presence of a liquid diluent (VII), is converted to caprolactam in the presence of a catalyst (V).
    • 提供了从式(I)化合物制备己内酰胺的方法:NC-(CH 2)5 -CO-R(I),其中R是羧酰胺,羧酸或羧酸酯基,其中a) 在氨和任选的液体稀释剂(VI)存在下,化合物(I)或这些化合物的混合物在氢气存在下在催化剂(II)的存在下氢化,得到混合物(III),b)氢 并将催化剂(II)与混合物(III)分离,得到混合物(Ⅳ),和c)任选在液体稀释剂(Ⅶ)存在下,混合物(Ⅳ)在存在下转化为己内酰胺 的催化剂(V)。
    • 7. 发明授权
    • Copper catalyzed process for producing 4-substituted azetidinone
derivatives
    • 用于生产4-取代的氮杂环丁酮衍生物的铜催化方法
    • US5808055A
    • 1998-09-15
    • US498499
    • 1995-07-05
    • Masashi Nakajima, deceasedYasuharu KimuraKiyohito Imai
    • Masashi Nakajima, deceasedYasuharu KimuraKiyohito Imai
    • C07D201/02C07D205/09C07D403/12C07D405/12C07F7/18
    • C07D403/12C07D201/02C07D205/09C07D405/12
    • A process for producing a 4-substituted azetidinone derivative represented by the following general formula �III!: ##STR1## (wherein OR is a protected hydroxy group, Y is an alkyl group, an alkoxy group, a silyloxy group, a carbamoyloxy group, an amino group, a substituted or unsubstituted aromatic group or a substituted or unsubstituted heterocyclic group, and n is an integer of 0 or 1, provided that n does not represent 0 when Y is an alkoxy group, silyloxy group, carbamoyloxy group or amino group), characterized in that a 2-azetidinone derivative represented by the following general formula �I!: ##STR2## (wherein OR is as defined above, and X is an alkyl group or a substituted or unsubstituted aromatic group) is reacted with thiocarboxylic acid represented by the following general formula �II!: HSCO--(CH.sub.2).sub.n --Y �II! (wherein Y and n are respectively as defined above) in an organic solvent in the presence of copper compounds.
    • 用于制备由以下通式[III]表示的4-取代的氮杂环丁酮衍生物的方法:其中OR为被保护的羟基,Y为烷基,烷氧基,甲硅烷氧基, 氨基甲酰氧基,氨基,取代或未取代的芳基或取代或未取代的杂环基,并且n为0或1的整数,条件是当Y为烷氧基时,n不为0,甲硅烷氧基,氨基甲酰氧基 或氨基),其特征在于由以下通式[I]表示的2-氮杂环丁酮衍生物:其中OR如上所定义,X为烷基或取代或未取代的芳族基团 )与铜化合物存在下的有机溶剂中由以下通式[II]表示的硫代羧酸反应:HSCO-(CH 2)n Y [II](其中Y和n分别如上定义)。
    • 9. 发明授权
    • Preparation of 5-membered ring heterocycles
    • 五元环杂环的制备
    • US5453516A
    • 1995-09-26
    • US165463
    • 1993-12-13
    • Rolf FischerRolf Pinkos
    • Rolf FischerRolf Pinkos
    • C07D201/02C07D207/26C07D207/267C07D307/33C07D315/00C07D207/27C07D307/28
    • C07D201/02C07D207/267C07D307/33C07D315/00
    • A process for preparing 5-membered ring heterocycles of the general formula I ##STR1## where R.sup.1 is methyl or hydroxyethyl,R.sup.2,R.sup.3,R.sup.4,R.sup.5 and R.sup.6 are hydrogen, C.sub.1 - to C.sub.12 -alkyl, C.sub.2 - to C.sub.12 -alkenyl, aryl, C.sub.3 - to C.sub.8 -cycloalkyl, C.sub.1 - to C.sub.12 -alkoxy, halogen, C.sub.2 - to C.sub.20 -alkoxycarbonylalkyl, C.sub.2 - to C.sub.20 -alkylcarbonyloxy, formyl, C.sub.2 - to C.sub.20 -formylalkyl, benzoyl or --CH(OR.sup.3)(OR.sup.5), or R.sup.3 and R.sup.5 together are a C.sub.2 - to C.sub.7 -alkylene chain which is unsubstituted or monosubstituted to pentasubstituted by R.sup.4 or a .dbd.CH--CH.dbd.CH--CH.dbd. unit which is unsubstituted or monosubstituted to tetrasubstituted by R.sup.4,X is oxygen or N--R.sup.4by reacting 5-membered ring heterocycles of the general formula II ##STR2## where R.sup.2, R.sup.3, R.sup.4, R.sup.5, R.sup.6 and X have the abovementioned meanings and Y is hydrogen, acetyl or C.sub.2 - to C.sub.20 -alkoxycarbonyl, with dimethyl or ethylene carbonate in the presence of a nitrogen-containing base at from 50.degree. to 300.degree. C. and from 0.01 to 50 bar is described.
    • 其中R 1是甲基或羟乙基,R 2,R 3,R 4,R 5和R 6是氢,C 1 -C 12 - 烷基,C 2 -C 12的通式I(I)的五元环杂环的制备方法 - 烯基,芳基,C 3 -C 8 - 环烷基,C 1 -C 12 - 烷氧基,卤素,C 2 -C 20 - 烷氧基羰基烷基,C 2 -C 20 - 烷基羰氧基,甲酰基,C 2 -C 20甲酰烷基,苯甲酰基或-CH )(OR 5)或R 3和R 5一起是未被取代或单取代以被R4或a = CH-CH = CH-CH =未被R4单取代或单取代的单元的C2至C7-亚烷基链, X是通过使通式II的5-元环杂环(II)其中R 2,R 3,R 4,R 5,R 6和X具有上述含义并且Y是氢,乙酰基或C 2 - 在含有50〜300℃的含氮碱和0.01〜50巴的存在下,与二甲基或碳酸亚乙酯进行反应。