Preparation of .epsilon.-caprolactone
    1.
    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 the production of 4-amino-6-tert.
butyl-3-mercapto-1,2,4-triazin-5-one
    4.
    发明授权
    Process for the production of 4-amino-6-tert. butyl-3-mercapto-1,2,4-triazin-5-one 失效
    制备4-氨基-6-叔丁氧基羰基的方法。 丁基-3-巯基-1,2,4-三嗪-5-酮

    公开(公告)号:US4326056A

    公开(公告)日:1982-04-20

    申请号:US266147

    申请日:1981-05-22

    IPC分类号: C07D253/06 C07D253/075

    CPC分类号: C07D253/075

    摘要: 4-amino-6-tert.butyl-3-mercapto-1,2,4-triazin-5-one of the formula ##STR1## is produced by reacting pivaloyl cyanide and isobutylene in the presence of acetic acid and sulfuric acid, hydrolyzing the reaction mixture in the presence of water and reacting the trimethyl pyruvic acid formed with thiocarbohydrazide. The triazinone is an important intermediate product in the synthesis of the known herbicide 4-amino-6-tert.butyl-3-methylmercapto-1,2,4-triazin-5-one.

    摘要翻译: 通过在乙酸和硫酸的存在下使新戊酰氰和异丁烯反应制备式“IMAGE”的4-氨基-6-叔丁基-3-巯基-1,2,4-三嗪-5-酮,水解 反应混合物在水存在下反应,并与硫代碳酰肼形成的三甲基丙酮酸反应。 三嗪酮是合成已知除草剂4-氨基-6-叔丁基-3-甲基巯基-1,2,4-三嗪-5-酮的重要中间产物。

    Process for the simultaneous production of 1,2- and 1,3-propanediol
    6.
    发明授权
    Process for the simultaneous production of 1,2- and 1,3-propanediol 失效
    同时生产1,2-和1,3-丙二醇的方法

    公开(公告)号:US5426249A

    公开(公告)日:1995-06-20

    申请号:US151389

    申请日:1993-11-12

    摘要: A process is described for the simultaneous production of 1,2- and 1,3-propanediol from glycerol. The process involves the reaction stages (a) dehydration of glycerol by feeding a gaseous glycerol-water mixture with 10 to 40 wt % glycerol at 250.degree. to 340.degree. C. over a solid catalyst with an H.sub.0 value (Hammett acidity function) of less than 2, preferably between -3 and -8.2, (b) hydration of the acrolein contained in the reaction mixture of stage (a), and (c) catalytic hydrogenation of the reaction mixture, containing 3-hydroxypropionaldehyde and hydroxyacetone, of stage (b). Two valuable products, namely 1,2- and 1,3-propanediol, can be obtained simultaneously and in high total yield from glycerol in a simple process.

    摘要翻译: 描述了从甘油同时生产1,2-和1,3-丙二醇的方法。 该方法包括反应阶段(a)通过在250℃至340℃下通过在H 2值(哈米特酸度函数)较小的固体催化剂上加入含有10至40重量%甘油的气态甘油 - 水混合物来脱水甘油 (b)使步骤(a)的反应混合物中所含的丙烯醛水合,(c)含有3-羟基丙醛和羟基丙酮的反应混合物的催化氢化 b)。 两个有价值的产物,即1,2-和1,3-丙二醇,可以在一个简单的过程中同时获得,并以高的总收率由甘油获得。

    Method for the recovery of aqueous solutions of free, neutral
.alpha.-amino acids from aqueous solutions of their alkali-metal salts
    10.
    发明授权
    Method for the recovery of aqueous solutions of free, neutral .alpha.-amino acids from aqueous solutions of their alkali-metal salts 失效
    从其碱金属盐的水溶液中回收游离的中性α-氨基酸的水溶液的方法

    公开(公告)号:US5049283A

    公开(公告)日:1991-09-17

    申请号:US483048

    申请日:1990-02-21

    CPC分类号: C07C227/16

    摘要: Aqueous solutions of free, neutral .alpha.-amino acids are recovered from aqueous solutions of their alkali-metal salts. Two equally large rectifying columns filled with a strongly acidic cation exchanger in the H.sup.+ form are used, the discharge of the first column being connected to the head of the second column. The solution of the alkali-metal salt is at first delivered to the head of the first column, then the residual solution, reduced by the alkali-metal cations adsorbed in the exchanger, is displaced to the second column by means of the addition of water. A product-free forerun is first separated at the discharge of the second column and, when free .alpha.-amino acid begins to exit in the flow-off from the second column, the receiver is changed and the delivery of water to the head of the first column continues further until a mixed pH between 5 and 7 has been achieved in the receiver. Then, the previously first column is decoupled and regenerated, the previously second column, which is now the first column, is coupled to a freshly regenerated column as second column and the entire process is repeated as often as desired.

    摘要翻译: 游离的中性α-氨基酸的水溶液从其碱金属盐的水溶液中回收。 使用填充有H +形式的强酸性阳离子交换器的两个同等大的精馏塔,第一塔的排放物连接到第二塔的头部。 首先将碱金属盐的溶液输送到第一塔的头部,然后通过吸附在交换器中的碱金属阳离子还原的残留溶液通过加入水而置换到第二塔 。 首先在第二柱的排出口处分离出无产物的前驱体,当游离的α-氨基酸在从第二塔的流出物中开始离开时,接收器被改变并且将水输送到 第一列继续进行,直到在接收器中达到5和7之间的混合pH。 然后,先前的第一列被解耦和再生,先前的第二列(现在是第一列)被耦合到作为第二列的新鲜再生的列,并且整个过程根据需要经常重复。