Process for the preparation of lysine
    1.
    发明授权
    Process for the preparation of lysine 失效
    制备LYSINE的方法

    公开(公告)号:US3681460A

    公开(公告)日:1972-08-01

    申请号:US3681460D

    申请日:1969-08-25

    Applicant: ALLIED CHEM

    Abstract: Lysine is produced by a process comprising the steps of 1. Nitrating cyclohexanone to form 2-nitrocyclohexanone; 2. Nitrosating the 2-nitrocyclohexanone to form 2-nitro-6oximinocyclohexanone; 3. Ring opening the 2-nitro-6-oximinocyclohexanone in alcoholic base to form an ester of 2-oximino-6-nitrocaproic acid; 4. Hydrogenating the 2-oximino-6-nitro caproic acid alkyl ester to form an alkyl ester of lysine; and 5. Saponifying the lysine alkyl ester to afford lysine or a salt thereof.

    Abstract translation: 赖氨酸通过包括以下步骤的方法制备:1.将环己酮硝化以形成2-硝基环己酮; 2.硝基化2-硝基环己酮形成2-硝基-6-肟基环己酮; 3.在醇基中打开2-硝基-6-肟基环己酮,形成2-肟基-6-硝基己酸的酯; 4.氢化2-肟基-6-硝基己酸烷基酯以形成赖氨酸的烷基酯; 皂化赖氨酸烷基酯以提供赖氨酸或其盐。

    Separation of {60 -amino-{107 -lactams from beckmann rearrangement mixtures
    2.
    发明授权
    Separation of {60 -amino-{107 -lactams from beckmann rearrangement mixtures 失效
    {60-氨基 - {107-内酰胺与贝克曼重排混合物的分离

    公开(公告)号:US3910891A

    公开(公告)日:1975-10-07

    申请号:US47713174

    申请日:1974-06-06

    Applicant: ALLIED CHEM

    CPC classification number: C07D223/12

    Abstract: A process provided for separating an Alpha -amino- omega lactam of the formula:

    WHEREIN N IS AN INTEGER FROM 0 TO 12, IN ITS FREE FORM FROM THE REARRANGED MIXTURE OBTAINED BY THE Beckmann rearrangement of an Alpha -aminocycloalkanone oxime of the formula:

    WHEREIN N IS AN INTEGER FROM 0 TO 12, WHICH PROCESS COMPRISES THE STEPS OF: CONTACTING THE REARRANGED MIXTURE WITH A SOLVENT SELECTED FROM THE GROUP CONSISTING OF: A. LINEAR AND CYCLIC ETHERS AND POLYETHERS, B. C3 to C8 alcohols in the absence of chloride ions, C. NITRILES CONTAINING TWO OR MORE CARBON ATOMS, D. AROMATICS AND HALOAROMATICS IN THE PRESENCE OF AT LEAST ONE OF SAID (A) OR (B), WHEREIN THE HALO SUBSTITUENT IS CHLORINE OR BROMINE AND IS ATTACHED DIRECTLY TO THE RING, E. CHLOROFORM, F. TRICHLOROETHYLENE IN THE PRESENCE OF AT LEAST ONE OF SAID (A) OR (B), AND G. MIXTURES OF TWO OR MORE OF THE ABOVE, WHILE SIMULTANEOUSLY NEUTRALIZING THE RESULTANT SOLUTION WITH AN EXCESS OF ANHYDROUS AMMONIA BASED ON THE HYDROGEN ION CONCENTRATION IN THE SOLUTION, WHEREBY AN INSOLUBLE AMMONIUM SALT PRECIPITATE IS FORMED; AND SEPARATING A SOLUTION CONTAINING AN Alpha -AMINO- omega -LACTAM IN ITS FREE FORM FROM THE PRECIPITATE.

    Abstract translation: 一种用于分离下式的α-氨基-ω-内酰胺的方法:

    Process for the production of 2-aminocycloalkanone oxime
    4.
    发明授权
    Process for the production of 2-aminocycloalkanone oxime 失效
    生产2-氨基环烷酮肟的方法

    公开(公告)号:US3917699A

    公开(公告)日:1975-11-04

    申请号:US42295273

    申请日:1973-12-07

    Applicant: ALLIED CHEM

    CPC classification number: C07C249/08

    Abstract: 2-Aminocycloalkanone oximes are produced by reacting, in an oxygen-free environment, hydroxylamine phosphate or hydroxylamine sulfate with anhydrous ammonia; removing the precipitated ammonium salt; adding ammonium chloride to the solution; maintaining the solution within a preselected temperature range while adding 2-chlorocycloalkanone; maintaining the desired temperature until the reaction is complete and isolating the oxime product.

    Abstract translation: 通过在无氧环境下使磷酸羟胺或硫酸羟胺与无水氨反应制备2-氨基环烷酮肟; 除去沉淀的铵盐; 向溶液中加入氯化铵; 将溶液保持在预选的温度范围内,同时加入2-氯环烷酮; 保持所需的温度直到反应完成并分离出肟产物。

    Nitro-oximino alkanoic acids as plant growth regulants
    5.
    发明授权
    Nitro-oximino alkanoic acids as plant growth regulants 失效
    硝基肟基链烷酸作为植物生长调节剂

    公开(公告)号:US3873301A

    公开(公告)日:1975-03-25

    申请号:US38705473

    申请日:1973-08-09

    Applicant: ALLIED CHEM

    CPC classification number: C07D333/36 A01N37/50

    Abstract: A method of improving the yield of plants such as legumes by the application thereto of plant growth regulants comprising nitrooximino alkanoic acids and derivatives thereof having the general formula:

    WHEREIN N IS AN INTEGER FROM 1 TO 12 AND WHEREIN Y is selected from the group consisting of OR, SR, NRR'' in which R and R'' are independently selected from the group consisting of hydrogen, alkyl, cycloalkyl, alkaryl, aralkyl, aryl, heterocyclic, alkenyl and alkynyl, and OR'''' in which R'''' is an alkali metal.

    Abstract translation: 一种通过应用植物生长调节剂来提高植物如豆类的产量的方法,所述植物生长调节剂包含硝基肟基链烷酸及其衍生物,其具有以下通式:

    Continuous process for preparing cumene hydroperoxide
    7.
    发明授权
    Continuous process for preparing cumene hydroperoxide 失效
    连续制备氢过氧化枯烯的方法

    公开(公告)号:US3907901A

    公开(公告)日:1975-09-23

    申请号:US34843073

    申请日:1973-04-05

    Applicant: ALLIED CHEM

    CPC classification number: C07C409/10 C07C407/00 C07C407/003 C07C409/14

    Abstract: An improved continuous process for preparing cumene hydroperoxide and phenol by the controlled liquid phase air oxidation of cumene in the absence of initiators, catalysts, additives or alkalizing agents. A mixture containing cumene having a purity of at least 99.8 percent, and recycle cumene hydroperoxide which has been purified by washing with aqueous alkali metal hydroxide, followed by water wash, is oxidized in a single or multiple stage system by continuously passing through the mixture a stream of gas containing at least 8 mol percent of oxygen at a rate wherein the ratio of the mols of oxygen supplied per hour to the maximum amount of oxygen consumable per hour exdeeds 0.25 and the exit gas contains from 3-10 percent oxygen; and when oxidation is effected in a mutiple stage system the temperature is maintained stepwise from about 120* to about 80*C. while the concentration of cumene hydroperoxide in the reaction mixture is permitted to increase stepwise from about 8 percent to about 40 percent.

    Abstract translation: 在不存在引发剂,催化剂,添加剂或碱化剂的情况下,通过异丙苯的受控液相空气氧化来制备氢过氧化异丙苯和苯酚的改进的连续方法。 含有纯度至少为99.8%的异丙基苯的混合物,以及通过用碱金属氢氧化物水溶液洗涤纯化,然后水洗后再循环的异丙基氢过氧化物,在单级或多级系统中通过连续通过混合物a 含有至少8mol%氧气的气体流,其中每小时供应的氧气摩尔数与每小时最大氧消耗量的比例超过0.25,出口气体含有3-10%的氧气; 并且当在多级系统中进行氧化时,温度从约120℃至约80℃逐步维持,而反应混合物中氢过氧化异丙苯的浓度允许从约8%至约40%逐步增加。

    Method of preparing an ' -amino-'7 -lactam
    8.
    发明授权
    Method of preparing an ' -amino-'7 -lactam 失效
    制备'-AMINO-7 -LACTAM的方法

    公开(公告)号:US3904610A

    公开(公告)日:1975-09-09

    申请号:US52628174

    申请日:1974-11-22

    Applicant: ALLIED CHEM

    CPC classification number: C07D223/12

    Abstract: There is provided an improved method of producing an Alpha amino- omega -lactam of the formula

    BY THE Beckmann rearrangement of an Alpha -aminocycloalkanone oxime of the formula

    WHEREIN N IS AN INTEGER BETWEEN 0 AND 12, THE IMPROVEMENT COMPRISING THE STEPS OF: 1. DISSOLVING, IN A FIRST REACTION STEP, THE OXIME OR A MIXTURE CONTAINING THE OXIME AND AN ACID SALT THEREOF, AND NH4Cl in sulfuric acid having a concentration of about 100 to 110% (i.e., water-free sulfuric acid containing up to 45% by weight of free SO3) while maintaining a temperature in the first reaction step in the range of about -5* to 35*C; 2. removing the evolved HCl gas formed in the first reaction step; 3. ADDING, IN A SECOND REACTION STEP THE SOLUTION FROM THE FIRST REACTION STEP TO SULFURIC ACID OF A CONCENTRATION OF ABOUT 100 TO 110% OR TO A Beckmann rearrangement mixture derived from said oxime containing sulfuric acid of such concentration while maintaining a temperature in said second reaction step below about 100*C by cooling, the rate of addition of the solution and the amount of cooling being adjusted to maintain the temperature in said range, whereby a rearrangement mixture is formed; 4. REMOVING THE EVOLVED HCl gas formed in the second reaction step; and 5. STRIPPING RESIDUAL HCl from the rearrangement mixture, whereby a lactam solution substantially free of HCl is formed.

    Process for the preparation of lysine
    9.
    发明授权
    Process for the preparation of lysine 失效
    制备LYSINE的方法

    公开(公告)号:US3876685A

    公开(公告)日:1975-04-08

    申请号:US20391471

    申请日:1971-12-01

    Applicant: ALLIED CHEM

    Abstract: Lysine is produced by a process comprising the steps of 1. Nitrating cyclohexanone to form 2-nitrocyclohexanone; 2. Nitrosating the 2-nitrocyclohexanone to form 2-nitro-6oximinocyclohexanone; 3. Ring opening the 2-nitro-6-oximinocyclohexanone in alcoholic base to form an ester of 2-oximino-6-nitrocaproic acid; 4. Hydrogenating the 2-oximino-6-nitro caproic acid alkyl ester to form an alkyl ester of lysine; and 5. Saponifying the lysine alkyl ester to afford lysine or a salt thereof.

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