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    • 1. 发明授权
    • Catalyst system for manufacturing p-chlorophenyl-N-methyl carbamate
    • 用于制备对氯苯基-N-甲基氨基甲酸酯的催化剂体系
    • US4390710A
    • 1983-06-28
    • US312207
    • 1981-10-19
    • James A. Manner
    • James A. Manner
    • C07C271/06C07D307/77C07C125/06C07D317/08
    • C07D307/77C07C271/06
    • Aromatic esters of carbamic acid derivatives, e.g., p-chlorophenyl-N-methyl carbamate, are prepared by reaction of the corresponding aromatic alcohol, e.g., p-chlorophenol, and monoisocyanate, e.g., methyl isocyanate, in the presence of a catalytic amount of a combination of a 4-aminopyridine catalyst, e.g., 4-dimethylaminopyridine, and pyridine or methyl substituted pyridines. The product is substantially pure, having less than 0.80 weight percent allophanate ester by-product, e.g., p-chlorophenyl-N,N'-dimethyl allophanate, and less than 0.50 weight percent unreacted aromatic alcohol, e.g., p-chlorophenol. The reaction is readily controlled and characterized by the substantial absence of reflux. The product can be retained in the liquid state at reaction temperature for extended periods of time without significantly increasing the level of allophanate ester by-product.
    • 氨基甲酸衍生物的芳族酯,例如对氯苯基-N-甲基氨基甲酸酯,通过相应的芳族醇例如对氯苯酚和单异氰酸酯例如甲基异氰酸酯在催化量的 4-氨基吡啶催化剂,例如4-二甲基氨基吡啶和吡啶或甲基取代的吡啶的组合。 该产品基本上是纯的,具有小于0.80重量%的脲基甲酸酯副产物,例如对氯苯基-N,N'-二甲基脲基甲酸酯和小于0.50重量%的未反应芳族醇,例如对氯苯酚。 反应容易控制,并且基本上没有回流而表征。 产物可以在反应温度下保持在液态较长时间,而不会显着提高脲基甲酸酯副产物的含量。
    • 2. 发明授权
    • Drying of dialkyl peroxydicarbonates
    • 干燥过氧化二碳酸二烷基酯
    • US4031126A
    • 1977-06-21
    • US657526
    • 1976-02-12
    • James A. Manner
    • James A. Manner
    • C07C407/00C07C68/08
    • C07C407/003
    • Dialkyl peroxydicarbonates are prepared in aqueous reaction media, washed with water, and then dried with sodium sulfate, calcium chloride, or the like. Peroxydicarbonates, particularly heat-sensitive peroxydicarbonates, may be dried safely and more effectively with the use of molecular sieves by contacting substantially phase water free peroxydicarbonate with sieves. Contact between heat-sensitive peroxydicarbonate and sieves should be effected in a way that avoids abrupt, excessive warming of peroxydicarbonate.
    • 在含水反应介质中制备过氧二碳酸二烷基酯,用水洗涤,然后用硫酸钠,氯化钙等进行干燥。 过氧碳酸氢盐,特别是热敏性过氧化二碳酸酯,可以通过使基本相不含水的过氧化二碳酸酯与筛子接触而使用分子筛安全地和更有效地干燥。 热敏过氧化二碳酸酯和筛子之间的接触应以避免过度二碳酸酯突然,过度升温的方式进行。
    • 5. 发明授权
    • Process for preparing N,O-disubstituted hydroxylamine compounds
    • 制备N,O-二取代羟胺化合物的方法
    • US5371264A
    • 1994-12-06
    • US9528
    • 1993-01-27
    • James A. MannerSuresh B. Damle
    • James A. MannerSuresh B. Damle
    • C07C239/22C07C269/04C07C271/00C07C275/64C07C69/96
    • C07C275/64C07C239/22C07C269/04C07C271/00
    • Describes a process for preparing N,O-disubstituted hydroxylamine compounds comprising reacting an aqueous solution of free hydroxylamine with an equimolar amount of a carbonyl halide-containing compound, e.g., a chloroformate such as phenyl chloroformate, in the presence of a substantially stoichiometric amount of a weak inorganic basic reagent, thereby to produce the N-substituted derivative, and thereafter further reacting an inert organic solvent solution of the N-substituted derivative with an equimolar amount of the corresponding carbonyl halide-containing compound in the presence of a substantially stoichiometric amount of weak inorganic basic reagent, thereby to produce the N,O-disubstituted derivative, e.g., N,O-bis(phenoxycarbonyl) hydroxylamine. In a preferred embodiment, the organic solvent is used also in the reaction that produces the N-substituted derivative. N,O-disubstituted hydroxylamine compounds containing less than 3 weight percent, e.g., less than 0.5 weight percent, of the hydrolysis by-product of the carbonyl halide-containing compound may be produced thereby.
    • 描述了制备N,O-二取代的羟胺化合物的方法,包括使游离羟胺的水溶液与等摩尔量的含羰基卤化合物,例如氯甲酸酯如氯甲酸苯酯,在基本上化学计量的 弱的无机碱性试剂,从而产生N-取代的衍生物,然后在基本上化学计量的存在下,使N-取代的衍生物的惰性有机溶剂溶液与等摩尔量的相应的含羰基卤化合物进一步反应 的弱无机碱性试剂,从而产生N,O-二取代的衍生物,例如N,O-双(苯氧基羰基)羟胺。 在优选的实施方案中,有机溶剂也用于产生N-取代的衍生物的反应中。 因此可以制备含有小于3重量%,例如小于0.5重量%的含羰基卤化合物的水解副产物的N,O-二取代羟胺化合物。