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    Continuous process for preparing cumene hydroperoxide
    12.
    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

    Inventor： FEDER RAYMOND L ,  FUHRMANN ROBERT ,  PISANCHYN JOHN ,  ELISHEWITZ SAUL ,  INSINGER THOMAS H ,  MATHEW CHEMPOLIL THOMAS

    IPC: C07C409/10 ,  C07C73/08

    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
    13.
    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

    Inventor： FUHRMANN ROBERT ,  PISANCHYN JOHN

    IPC: C07D223/12 ,  C07D207/26 ,  C07D211/76

    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
    14.
    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

    Inventor： PISANCHYN JOHN ,  FUHRMANN ROBERT ,  SIFNIADES STYLIANOS ,  TUNICK ALLEN ABRAHAM

    IPC: C07C101/54

    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.

    Resolution of lysineamide
    15.
    发明授权
    Resolution of lysineamide 失效
    赖氨酸的分解

    公开(公告)号：US3862985A

    公开(公告)日：1975-01-28

    申请号：US39110073

    申请日：1973-08-27

    Applicant: ALLIED CHEM

    Inventor： SIFNIADES STYLIANOS ,  FUHRMANN ROBERT ,  TUNICK ALLEN A

    IPC: C07C237/00 ,  C07D207/28 ,  C07C103/00

    CPC classification number: C07D207/28 ,  C07C237/00

    Abstract: L-lysineamide dihydrochloride can be isolated by preparing the intermediate D- and L-lysineamide-L-pyrrolidone carboxylate hydrochloride salts which can be separated from alkanol solution by fractional crystallization. The L-lysineamide pyrrolidone carboxylate hydrochloride salt is then treated with excess hydrogen chloride to form the desired L-lysineamide dihydrochloride.

    Abstract translation: 可以通过制备中间体D-和L-赖氨酰胺-L-吡咯烷酮羧酸盐酸盐盐分离L-赖氨酰胺二盐酸盐，其可以通过分级结晶与烷醇溶液分离。 然后用过量的氯化氢处理L-赖氨酰胺吡咯烷酮羧酸盐酸盐，形成所需的L-赖氨酰胺二盐酸盐。

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