专利号:US-6696590-B2 优先权日:2000-12-22 标题 :Process for the synthesis of aliphatic, cycloaliphatic or araliphatic chloroformates 发明人:BONNARD HUBERT; FERRUCCIO LAURENCE; GAUTHIER PATRICIA; SENET JEAN-PIERRE 权利人:POUDRES & EXPLOSIFS STE NALE 摘要:The disclosure relates to a process for the synthesis of substituted or unsubstituted aliphatic, cycloaliphatic or araliphatic chloroformates by reaction of the corresponding alcohol with phosgene, diphosgene and/or triphosgene. The reaction is carried out under a pressure of between 15×10 3 Pa and 85×10 3 Pa and at a temperature of between −30° C. and +50° C. The process is particularly well suited to the preparation of menthyl chloroformate and benzyl chloroformate.
专利号:US-5654485-A 优先权日:1996-03-25 标题:Synthesis of cycloalkyldiarylphosphines 发明人:SENARATNE K PUSHPANANDA A; MALCOLM ARCELIO J; ORIHUELA FELIX M; ELNAGAR HASSAN Y 权利人:ALBEMARLE CORP 摘要:By reacting certain partially sterically-hindered chloro-substituted cycloalkanes with sodium and/or potassium diarylphosphides in an ether reaction medium, not only are useful cycloalkyldiarylphosphines produced, but in addition the chloro-substituted cycloalkane does not undergo any appreciable reaction with the coproduced aryl sodium and/or aryl potassium as it is formed. Moreover, the process makes it possible to avoid or at least to greatly reduce interaction with or cleavage of cyclic ether reaction media such as tetrahydrofuran. Thus the process makes possible improvements both in yield and quality of the cycloalkyldiarylphosphite product. A two-stage process conducted in an ether reaction medium is also described. In the first stage the sodium and/or potassium diarylphosphine reactant is produced by reaction between sodium and/or potassium and triarylphosphine.
专利号:US-4366317-A 优先权日:1981-06-22 标题 :Process for synthesis of N-(hydrocarbyl)substituted-p-menthane-3-carboxamide 发明人:HAUT STEPHEN A; COMES ROGER A 权利人:PHILIP MORRIS INC 摘要:This invention provides an improved process for synthesizing carboxamides which involves reacting 3-p-menthyl halide with magnesium to form 3-p-menthylmagnesium halide Grignard reagent, and reacting the Grignard reagent with hydrocarbyl isocyanate at a temperature below about -20 DEG C. to form N-hydrocarbyl-p-menthane-3-carboxamide product. The product comprises a mixture of geometric isomers in which the 3-p-menthyl:3-p-neomenthyl weight ratio is at least 4:1 and can be as high as 9:1 under optimal conditions. This invention also provides a novel process for producing acylurea compounds such as N-(3-p-menthylcarbonyl)-N-t-butyl-N'-t-butylurea.
专利号:US-6020284-A 优先权日:1997-04-25 标 题:Preparation of Lucas reagent of enhanced utility and its use in synthesis of cycloaliphatic chlorides 发明人:SENARATNE K PUSHPANANDA A; ORIHUELA FELIX M; MALCOLM ARCELIO J 权利人:ALBEMARLE CORP 摘要:Gaseous anhydrous hydrogen chloride is introduced into an aqueous solution of zinc chloride under conditions effective to produce a more efficient Lucas reagent than a Lucas reagent made by mixing solid, anhydrous zinc chloride with 38% hydrochloric acid. For example, the reaction rate of such Lucas reagent with levo-menthol is much faster and requires a much shorter reaction period than Lucas reagent formed in the conventional manner from anhydrous, solid zinc chloride and concentrated (38%) hydrochloric acid. Also, the conversion to levo-menthyl chloride was higher when using Lucas reagent formed using gaseous anhydrous hydrogen chloride and aqueous zinc chloride solution. Also, Lucas reagent made in this manner is highly amenable to recycling, and requires only addition thereto of hydrogen chloride to replenish the catalyst for an ensuing run.
专利号:US-5654486-A 优先权日:1996-03-25 标题 :Synthesis of cycloalkyldiarylphosphines 发明人:SENARATNE K PUSHPANANDA A; MALCOLM ARCELIO J; ORIHUELA FELIX M; ELNAGAR HASSAN Y 权利人:ALBEMARLE CORP 摘要:Partially sterically-hindered cycloalkyl chlorides are reacted with lithium diarylphosphides in inert liquid hydrocarbon reaction media to form cycloalkyldiarylphosphines. Aryl lithium is coproduced. The process makes it possible to avoid, or at least substantially eliminate, the interaction with or cleavage of cyclic ether reaction media such as tetrahydrofuran, previously the solvent of choice for conducting this type of reaction. Also during the conduct of the present process the chloro-substituted cycloalkane does not undergo any appreciable reaction with the coproduced aryl lithium as it is formed. Thus improvements both in yield and quality of the cycloalkyldiarylphosphine product are made possible. A comprehensive three-step process for converting triarylphosphine to cycloalkyldiarylphosphine is also described.
专利号:US-5856597-A 优先权日:1997-04-25 标题 :Preparation of lucas reagent of enhanced utility and its use in synthesis of cycloaliphatic chlorides