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    • 5. 发明授权
    • Production of ketazines
    • 生产酮类
    • US3965097A
    • 1976-06-22
    • US556036
    • 1975-03-06
    • Kurt-Wilhelm EichenhoferReinhard Schliebs
    • Kurt-Wilhelm EichenhoferReinhard Schliebs
    • C07C251/88C07C67/00C07C241/00C07C109/00
    • C07C251/88Y02P20/582
    • A process for the production of a ketazine of the general formula ##EQU1## in which R.sub.1, R.sub.2, R.sub.3 and R.sub.4 each independently is an alkyl, cycloalkyl or aralkyl radical with up to 12 carbon atoms; or an optionally substituted aryl radical with up to 10 carbon atoms, at most two of the radicals R.sub.1, R.sub.2, R.sub.3 and R.sub.4 being aryl radicals, orR.sub.1 + r.sub.2 and R.sub.3 + R.sub.4 individually is an alkylene radical with from 5 to 10 carbon atoms,Which comprises reacting a 3,3-diorganyl oxaziridine of the formula ##EQU2## with ammonia in the presence of a ketone of the formula ##EQU3## Advantageously the oxaziridine is 3,3-dimethyl oxaziridine, 3,3-methyl ethyl oxaziridine, 3,3-diethyl oxaziridine or 3,3-pentamethylene oxaziridine, the ketone is acetone, methyl ethyl ketone, diethyl ketone or cyclohexanone, the ammonia is used in gaseous form or in solution in water, and the reaction is carried out at a temperature of about -20 to 100.degree.C at a pressure ranging from about normal up to an excess pressure of about 10 atmospheres in a solvent selected from the group consisting of hydrocarbons with up to 12 carbon atoms, lower chlorinated hydrocarbons, halogenated derivatives of benzene, and alcohols with from 5 to 10 carbon atoms.
    • 制备通式为R 1 R 3的酮连氮的方法,其中R 1,R 2,R 3和R 4各自独立地为具有至多12个碳原子的烷基,环烷基或芳烷基; 或具有至多10个碳原子的任选取代的芳基,基团R 1,R 2,R 3和R 4中至多两个为芳基,或者R 1 + R 2和R 3 + R 4分别为具有5至10个碳原子的亚烷基 其包含在式R 3的酮存在下与氨反应制备式R1NH ANGLE C ANGLE | R2O的3,3-二异恶唑烷酮有利的是,氮杂氮丙啶是3,3-二甲基恶唑烷,3, 3-甲基乙基恶唑烷,3,3-二乙基恶唑烷或3,3-五亚甲基恶唑烷,酮是丙酮,甲基乙基酮,二乙基酮或环己酮,氨以气态或水溶液形式使用,反应 在大约-20至100℃的温度下,在大约正常的压力范围内,在约10个大气压的过压下,在选自碳原子数12个碳原子的溶剂中,低级氯代烃 ,苯的卤代衍生物 烯和具有5至10个碳原子的醇。
    • 7. 发明授权
    • Working up synthesis solutions obtained in production of hydrazine
    • 处理肼生产中得到的合成溶液
    • US4005179A
    • 1977-01-25
    • US597263
    • 1975-07-18
    • Kurt-Wilhelm EichenhoferReinhard SchliebsHermann BrandlHeinrich Kohnen
    • Kurt-Wilhelm EichenhoferReinhard SchliebsHermann BrandlHeinrich Kohnen
    • C01B21/16C07C67/00C07C241/00C07C251/88
    • C01B21/16C07C241/02C07C249/16
    • In the production of hydrazine wherein aqueous ammonia is oxidized in the presence of a ketone to form an aqueous solution containing at least one of a hydrazone and a ketazine along with ammonia, the hydrazone and ketazine are concentrated and the hydrazone and ketazine are subsequently hydrolyzed to hydrazine and ketone, the improvement which comprises effecting the concentration of the hydrazone and ketazine by extracting the aqueous solution with a substantially water-immiscible organic solvent whereby the hydrazone and ketazine preferentially enter the water-immiscible solvent, and separating the water-immiscible solvent extract from the aqueous solution. The organic solvent is preferably a higher alcohol, a chlorinated hydrocarbon, benzene or a substitution product thereof. The organic solvent extract, in one or more stages, and optionally with addition of ketone, can be re-extracted with water, hydrolyzed with aqueous acid or subjected to distillation to separate the hydrazine values from the organic solvent.
    • 在肼的制备中,其中氨在酮的存在下被氧化以形成含有腙和酮连氮中的至少一种的水溶液以及氨,腙和酮连氮被浓缩,腙和酮连接被水解成 肼和酮的改进,其包括通过用基本上与水不混溶的有机溶剂萃取水溶液来实现腙和酮连氮的浓度,由此腙和酮连接优先进入与水不混溶的溶剂,并且将水不混溶的溶剂萃取物 从水溶液中。 有机溶剂优选为高级醇,氯代烃,苯或其取代产物。 在一个或多个阶段中,有机溶剂提取物和任选地加入酮可以用水重新萃取,用酸水溶液或进行蒸馏以将肼值与有机溶剂分离。
    • 10. 发明授权
    • Production of 3,4-dihydroxy phospholane oxides
    • 3,4-二羟基磷酰氧化物的生产
    • US4102949A
    • 1978-07-25
    • US758527
    • 1977-01-11
    • Reinhard SchliebsHans-Dieter Block
    • Reinhard SchliebsHans-Dieter Block
    • C07F9/36C07F9/6568C07F9/32C07F9/53
    • C07F9/36C07F9/65681C07F9/65685
    • A process for the preparation of a 3,4-dihydroxy phsopholane oxide of the formula ##STR1## in which R.sup.1 represents an alkyl, alkoxy, alkenyl, alkenyloxy, alkinyl or alkinyloxy with up to 18 carbon atoms and substitution products thereof; aryl and aryloxy having up to 14 carbon atoms and substitution products thereof; cycloalkyl and cycloalkoxy having up to 6 ring carbon atoms and substitution products thereof; dialkylamino having up to 6 carbon atoms per alkyl radical and substitution products thereof; and N-hetero-radicals, andR.sup.2, r.sup.3 and R.sup.4 independently of one another represent a C.sub.1 -C.sub.4 -alkyl radical or hydrogen,Comprising reacting a phospholene oxide of the formula ##STR2## with hydrogen peroxide in the presence of a catalytic amount of an osmium compound at a temperature in the range of about 20.degree. to 150.degree. C, especially about 35.degree. to 100.degree. C.
    • 制备式“IMAGE”的3,4-二羟基环己烷氧化物的方法,其中R 1表示具有至多18个碳原子的烷基,烷氧基,烯基,烯氧基,炔基或烷氧基及其取代产物; 具有至多14个碳原子的芳基和芳氧基及其取代产物; 环烷基和具有至多6个环碳原子的环烷氧基及其取代产物; 每个烷基具有至多6个碳原子的二烷基氨基及其取代产物; 和N-杂原子,R 2,R 3和R 4彼此独立地表示C 1 -C 4 - 烷基或氢,在过氧化氢的存在下,在催化量的 锇化合物在约20至150℃,特别是约35至100℃的温度范围内。