Process for the manufacture of a gamma-halotiglic aldehyde
    1.
    发明授权
    Process for the manufacture of a gamma-halotiglic aldehyde 失效
    制备γ-卤代醛的方法

    公开(公告)号:US5786518A

    公开(公告)日:1998-07-28

    申请号:US904523

    申请日:1997-08-01

    摘要: A novel process for the manufacture of a .gamma.-halotiglic aldehyde HalH.sub.2 C--CH.dbd.C(CH.sub.3)--CHO �I!, wherein Hal signifies chlorine or bromine, comprises haloalkoxylating a 1-alkoxy-2-methyl-1,3-butadiene H.sub.2 C.dbd.CH--C(CH.sub.3).dbd.CH--OR.sup.1 �II!, wherein R.sup.1 signifies C.sub.1-4 -alkyl, using a particular halogenating agent in a C.sub.1-4 -alkanol (R.sup.2 OH) and hydrolyzing the thus-obtained .gamma.-halotiglic aldehyde dialkyl acetal HalH.sub.2 C--CH.dbd.C(CH.sub.3)--CH(OR.sup.1)(OR.sup.2) �III! to the desired .gamma.-chloro- or .gamma.-bromotiglic aldehyde I. The halogenating agent used in this process is selected from an alkali metal hypochlorite, an alkali metal hypobromite, an alkaline earth metal hypochlorite, an alkaline earth metal hypobromite, tert.butyl hypochlorite, N-bromoacetamide, 1.3-dichloro-5,5-dimethylhydantoin and 1,3-dibromo-5,5-dimethylhydantoin. Further aspects of the present invention are the use of the thus-manufactured .gamma.-halotiglic aldehyde for the production of .gamma.-acetoxy-tiglic aldehyde or of a Wittig aldehyde halide Hal-Ph.sub.3 P.sup.+ CH.sub.2 --CH.dbd.C(CH.sub.3)--CHO �VII!, wherein Hal signifies chlorine or bromine and Ph signifies phenyl, as well as a process for the catalytic dealkoxylation of the 1,1,3-trialkoxy-2-methyl-butane CH.sub.3 --CH(OR.sup.1)--CH(CH.sub.3)--CH(OR.sup.1).sub.2 �VI! to the corresponding 1-alkoxy-2-methyl-1,3-butadiene II in the gas phase using an aluminium silicate of medium specific surface as the catalyst. The products I, .gamma.-acetoxy-tiglic aldehyde and VII are known, important intermediates for the production of various apocarotenoids and diapocarotenoids as well as of Vitamin A.

    摘要翻译: 用于制备γ-卤代醛HalH2C-CH = C(CH3)-CHO [I]的新方法,其中Hal表示氯或溴,包括1-烷氧基-2-甲基-1,3-丁二烯H 2 C的卤代烷氧基化 = CH-C(CH 3)= CH-OR 1 [II],其中R 1表示C 1-4 - 烷基,使用特定的卤化剂在C 1-4链烷醇(R 2 OH)中并水解由此得到的γ-卤代二烷基 缩醛HalH2C-CH = C(CH3)-CH(OR1)(OR2)[III]到所需的γ-氯 - 或γ-溴代醛I.本方法中使用的卤化剂选自碱金属次氯酸盐, 碱金属次溴酸盐,碱土金属次氯酸盐,碱土金属次溴酸盐,叔丁基次氯酸盐,N-溴乙酰胺,1,3-二氯-5,5-二甲基乙内酰脲和1,3-二溴-5,5-二甲基乙内酰脲。 本发明的其它方面是使用如此制备的γ-卤代醛用于制备γ-乙酰氧基 - 四氢呋喃或维蒂希醛卤化物Hal-Ph 3 P + CH 2 -CH = C(CH 3)-CHO [VII ],其中Hal表示氯或溴,Ph表示苯基,以及1,1,3-三烷氧基-2-甲基 - 丁烷CH3-CH(OR1)-CH(CH3)-CH(CH)的催化脱烷基化方法 (OR1)2 [VI]与相应的1-烷氧基-2-甲基-1,3-丁二烯II在气相中使用中等比表面积的硅酸铝作为催化剂。 产物I,γ-乙酰氧基 - lic醛和Ⅶ是已知的,用于生产各种类胡萝卜素和二糖皮质素以及维生素A的重要中间体。

    Process for the catalytic dealkoxylation of
1,1,3-trialkoxy-2-methyl-butane
    3.
    发明授权
    Process for the catalytic dealkoxylation of 1,1,3-trialkoxy-2-methyl-butane 失效
    1,1,3-三烷氧基-2-甲基 - 丁烷的催化脱烷基化方法

    公开(公告)号:US5990360A

    公开(公告)日:1999-11-23

    申请号:US76772

    申请日:1998-05-12

    摘要: A novel process for the manufacture of a .gamma.-halotiglic aldehyde HalH.sub.2 C-CH.dbd.C(CH.sub.3)-CHO [I], wherein Hal signifies chlorine or bromine, comprises haloalkoxylating a 1-alkoxy-2-methyl-1,3-butadiene H.sub.2 C.dbd.CH-C (CH.sub.3).dbd.CH-OR.sup.1 [II], wherein R.sup.1 signifies C.sub.1-4 -alkyl, using a particular halogenating agent in a C.sub.1-4 -alkanol (R.sup.2 OH) and hydrolyzing the thus-obtained .gamma.-halotiglic aldehyde dialkyl acetal HalH.sub.2 C-CH.dbd.C(CH.sub.3)-CH (OR.sup.1)(OR.sup.2) [III] to the desired .gamma.-chloro- or .gamma.-bromotiglic aldehyde I. The halogenating agent used in this process is selected from an alkali metal hypochlorite, an alkali metal hypobromite, an alkaline earth metal hypochlorite, an alkaline earth metal hypobromite, tert.butyl hypochlorite, N-bromoacetamide, 1.3-dichloro-5,5-dimethylhydantoin and 1,3-dibromo-5,5-dimethylhydantoin. Further aspects of the present invention are the use of the thus manufactured .gamma.-halotiglic aldehyde for the production of .gamma.-acetoxy-tiglic aldehyde or of a Wittig aldehyde halide Hal-Ph.sub.3 P.sup.+ CH.sub.2 -CH.dbd.C(CH.sub.3)-CHO [VII], wherein Hal signifies chlorine or bromine and Ph a process for the catalytic dealkoxylation of the 1,1,3-trialkoxy-2-methyl-butane CH.sub.3 -CH(ORl)-CH(CH.sub.3)-CH(OR.sup.1).sub.2 [VI] to the corresponding 1-alkoxy-2-methyl-1,3-butadiene II in the gas phase using an aluminium silicate of medium specific surface as the catalyst. The products I, .gamma.-acetoxy-tiglic aldehyde and VII are known, important intermediates for the production of various apocarotenoids and diapocarotenoids as well as of Vitamin A.

    摘要翻译: 用于制备γ-卤代醛HalH2C-CH = C(CH3)-CHO [I]的新方法,其中Hal表示氯或溴,包括1-烷氧基-2-甲基-1,3-丁二烯H 2 C的卤代烷氧基化 = CH-C(CH 3)= CH-OR 1 [II],其中R 1表示C 1-4 - 烷基,使用特定的卤化剂在C 1-4链烷醇(R 2 OH)中并水解由此得到的γ-卤代二烷基 缩醛HalH2C-CH = C(CH3)-CH(OR1)(OR2)[III]到所需的γ-氯 - 或γ-溴代醛I.本方法中使用的卤化剂选自碱金属次氯酸盐, 碱金属次溴酸盐,碱土金属次氯酸盐,碱土金属次溴酸盐,叔丁基次氯酸盐,N-溴乙酰胺,1,3-二氯-5,5-二甲基乙内酰脲和1,3-二溴-5,5-二甲基乙内酰脲。 本发明的其它方面是使用如此制备的γ-卤代醛用于制备γ-乙酰氧基 - 四氢呋喃或维蒂希醛卤化物Hal-Ph 3 P + CH 2 -CH = C(CH 3)-CHO [VII] 其中Hal表示氯或溴,Ph表示1,1,3-三烷氧基-2-甲基 - 丁烷CH 3 -CH(OR 1)-CH(CH 3)-CH(OR 1)2 [VI]的催化脱烷基化方法, 使用中等比表面积的硅酸铝作为催化剂,在气相中与相应的1-烷氧基-2-甲基-1,3-丁二烯II反应。 产物I,γ-乙酰氧基 - lic醛和Ⅶ是已知的,用于生产各种类胡萝卜素和二糖皮质素以及维生素A的重要中间体。

    Process for preparing 5-cyano-4-methyl-oxazole
    4.
    发明授权
    Process for preparing 5-cyano-4-methyl-oxazole 失效
    制备5-氰基-4-甲基 - 恶唑的方法

    公开(公告)号:US4772718A

    公开(公告)日:1988-09-20

    申请号:US922596

    申请日:1986-10-24

    申请人: Paul Nosberger

    发明人: Paul Nosberger

    CPC分类号: C07D263/34

    摘要: A process for the manufacture of 5-cyano-4-methyl-oxazole which comprises reacting a 5-(lower alkoxycarbonyl)-4-methyl-oxazole with ammonia in the gaseous phase, in the presence of a zirconium oxide or hafnium oxide catalyst.

    摘要翻译: 一种制备5-氰基-4-甲基恶唑的方法,其包括在氧化锆或氧化铪催化剂的存在下,使5-(低级烷氧羰基)-4-甲基 - 恶唑与气相中的氨反应。

    Method of making ascorbyl monophosphates
    5.
    发明授权
    Method of making ascorbyl monophosphates 失效
    制备抗坏血酸单磷酸酯的方法

    公开(公告)号:US6063937A

    公开(公告)日:2000-05-16

    申请号:US40210

    申请日:1998-03-17

    IPC分类号: A23L33/15 C07F9/655 C07F9/06

    CPC分类号: C07F9/65515

    摘要: The present invention provides a method of making alkali metal and alkaline earth metal salts of L-ascorbic acid 2-monophosphate comprising reacting a L-ascorbic acid 2-polyphosphate under alkaline conditions with an alkali metal or alkaline earth metal salt of L-ascorbic-acid in concentrated aqueous solution. The amount of the L-ascorbic acid salt is in molar excess of the polyphosphate and the pH value of the reaction medium is maintained in the range of from about 8 to about 11 wherein the reaction is carried out until substantially all of the polyphosphate has been consumed and only L-ascorbic acid 2-monophosphate salt is present. A further aspect of the present invention comprises spray drying the mixture obtained after completion of the reaction, cooling and dilution to a suitable viscosity. The product of the process according to the invention is suitable as an additive for human and animal foodstuffs; it is especially stable against oxidative and thermal degradation and has an especially high content of L-ascorbic acid monophosphate vis-a-vis polyphosphates and is accordingly primarily of use preferably for the nutritional enrichment of fish feed.

    摘要翻译: 本发明提供一种制备L-抗坏血酸2-单磷酸的碱金属和碱土金属盐的方法,其包括在碱性条件下使L-抗坏血酸2-多磷酸酯与L-抗坏血酸的碱金属或碱土金属盐反应, 酸在浓缩水溶液中。 L-抗坏血酸盐的量与多磷酸盐摩尔过量,反应介质的pH值保持在约8至约11的范围内,其中进行反应直到基本上所有的多磷酸盐已经被 并且仅存在L-抗坏血酸2-单磷酸盐。 本发明的另一方面包括将反应完成后获得的混合物喷雾干燥,冷却和稀释至合适的粘度。 本发明方法的产品适用于人和动物食品的添加剂; 它对氧化和热降解特别稳定,并且具有特别高含量的L-抗坏血酸单磷酸酯vis-+ E,gra a + EE -vis多磷酸盐,因此主要用于鱼饲料的营养富集。

    Process for manufacturing 5-cyano-4-lower alkyloxazoles
    6.
    发明授权
    Process for manufacturing 5-cyano-4-lower alkyloxazoles 失效
    制备5-氰基-4-低级烷氧基硅烷的方法

    公开(公告)号:US5214162A

    公开(公告)日:1993-05-25

    申请号:US803004

    申请日:1991-12-05

    申请人: Paul Nosberger

    发明人: Paul Nosberger

    CPC分类号: C07D263/34

    摘要: The invention is concerned with a process for the manufacture of 5-cyano-4-lower alkyl-oxazoles by dehydrating a 5-carbamoyl-4-lower alkyl-oxazole in the gas phase in the presence of a heterogeneous catalyst based on silicon dioxide and in the presence of an inert solvent. The heterogeneous catalyst used is formed SiO.sub.2 or SiO.sub.2 doped with an oxide of V, Mo, Fe, Co and/or Zn. An N-lower alkyl-pyrrolidone is preferably used as the inert solvent.

    摘要翻译: 本发明涉及通过在基于二氧化硅的多相催化剂存在下,在气相中脱水5-氨基甲酰基-4-低级烷基 - 恶唑来制备5-氰基-4-低级烷基 - 恶唑的方法,以及 在惰性溶剂的存在下。 使用的非均相催化剂形成掺杂有V,Mo,Fe,Co和/或Zn的氧化物的SiO 2或SiO 2。 优选使用N-低级烷基吡咯烷酮作为惰性溶剂。

    Process for manufacture of beta-isophorone
    7.
    发明授权
    Process for manufacture of beta-isophorone 失效
    β-异佛尔酮的制造方法

    公开(公告)号:US5276197A

    公开(公告)日:1994-01-04

    申请号:US944027

    申请日:1992-09-11

    IPC分类号: B01J23/755 C07C45/67

    CPC分类号: B01J23/755 C07C45/67

    摘要: The invention is concerned with a process for the manufacture of beta-isophorone from alpha-isophorone by converting alpha-isophorone into beta-isophorone in the presence of a heterogeneous catalyst in the gas phase. The heterogenous catalyst used is especially an oxide or mixed oxide of the elements Mg, Al, Si and Ni.

    摘要翻译: 本发明涉及通过在气相中存在非均相催化剂将α-异佛尔酮转化为β-异佛尔酮,从α-异佛尔酮制备β-异佛尔酮的方法。 所用的异质催化剂特别是元素Mg,Al,Si和Ni的氧化物或混合氧化物。

    Process for manufacturing a diketone
    8.
    发明授权
    Process for manufacturing a diketone 失效
    制造二酮的方法

    公开(公告)号:US4904805A

    公开(公告)日:1990-02-27

    申请号:US682123

    申请日:1984-12-17

    申请人: Paul Nosberger

    发明人: Paul Nosberger

    CPC分类号: C07D307/60

    摘要: A process for the manufacture of ketopantolactone of the formula ##STR1## from pantolactone, which comprises dehydrogenating pantolactone in the presence of a vanadium oxide-containing or molybdenum oxide-containing catalyst with oxygen or an oxygen-containing gas in the gas phase.

    摘要翻译: 本发明涉及一种从全内推式制备式“酮”酮的方法,该方法包括在含有氧化钒或含氧化钼的催化剂存在下,在气相中用氧或含氧气体脱氢泛酸内酯。