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    • 51. 发明授权
    • Process for preparing the sex pheromone of Lymantria dispar L
    • 制备Lymantria dispar L的性信息素的方法
    • US5677155A
    • 1997-10-14
    • US547926
    • 1995-10-25
    • Eiichiro FukusakiTetsuo OmataShuji Senda
    • Eiichiro FukusakiTetsuo OmataShuji Senda
    • C12P7/04A01N43/44C07D303/04C07D303/14C07D303/16C12P17/02C12P41/00C12P7/00C12N9/14C12N9/20
    • C07D303/14C07D303/04C07D303/16C12P17/02C12P41/004
    • A process for preparing the sex pheromone of Lymantria dispar L. effectively which comprises the steps of reacting 1-bromodecane and propargyl alcohol tetrahydropyranylether in the presence of sodium hydroxide to give 1-tetrahydropyranyloxy-2-tridecyne, treating the tetrahydropyranyloxy-2-tridecyne with p-toluenesulfonic acid to give 2-tridecyn-1-ol, catalystic-hydrogenating the 2-tridecyn-1-ol in the presence of Lindlar catalyst to give (Z)-2-tridecen-1-ol, oxidizing the (Z)-2-tridecen-1-ol with peroxide to give (.+-.)-cis-2,3-epoxy-1-tridecanol, reacting the (.+-.)-cis-2,3-epoxy-1-tridecanol with acid anhydride in the presence of hydrolase in an organic solvent for a stereoselective acylation and recovering unreacted optically active (2R, 3S)-cis-2,3-epoxy-1-tridecanol after the acylation, reacting the optically active (2R, 3S)-cis-2,3-epoxy-1-tridecanol with toluenesulfonylchloride to give (2R, 3S)-cis-1-p-toluenesulfoxy-2,3-epoxytridecane, and reacting the (2R, 3S)-cis-1-p-toluenesulfoxy-2,3-epoxytridecane with di(4-methylpentyl) lithium copper reagent to yield (7R, 8S)-cis-2-methyl-7,8-epoxyoctadecane which is the sex pheromone of Lymantria dispar L.
    • 一种用于制备Lymantria dispar L.的性信息素的方法,其包括在氢氧化钠存在下使1-溴癸烷和炔丙醇四氢吡喃基醚反应,得到1-四氢吡喃氧基-2-三癸基,用四氢吡喃氧基-2-三癸基 对甲苯磺酸,得到2-三癸基-1-醇,在Lindlar催化剂存在下催化氢化2-三癸基-1-醇,得到(Z)-2-十三碳烯-1-醇,氧化(Z) (+/-) - 顺式-2,3-环氧-1-十三烷醇,使(+/-) - 顺式-2,3-环氧-1-十三烷醇与 酸酐在水解酶存在下在有机溶剂中进行立体选择性酰化,并在酰化后回收未反应的光学活性(2R,3S) - 顺式-2,3-环氧-1-十三烷醇,使光学活性(2R,3S) - 顺式-2,3-环氧-1-十三烷醇与甲苯磺酰氯反应,得到(2R,3S) - 顺式-1-对甲苯磺酰-2,3-环氧十三烷,并使(2R,3S) - 顺式-1- -toluenesul (4-甲基戊基)锂铜试剂,得到(7R,8S) - 顺式-2-甲基-7,8-环十八烷,是Lymantria dispar L的性信息素。
    • 52. 发明授权
    • Dispersions of epoxy scavengers exhibiting improved raw stock keeping
    • 环氧清除剂的分散体表现出改善的原料保存
    • US5620632A
    • 1997-04-15
    • US427763
    • 1995-04-25
    • Krishnan Chari
    • Krishnan Chari
    • C07D303/16C07D303/22C07D303/34C07D303/42C07D303/46C07D405/12C07F5/02C07F9/655G03C1/005G03C7/392B01J13/00C08K5/524C09K15/26
    • C07D303/22C07D303/16C07D303/34C07D303/42C07D303/46C07D405/12C07F5/025C07F9/65502G03C1/005G03C7/39268G03C7/39296Y10S516/928
    • A process for preparing a solid particle dispersion of an epoxy compound of the formula SI, ##STR1## wherein R is H, an alkyl group, or an aryl group; L.sub.1 is an alkylene group or an arylene group; L.sub.2 is --O--, --CO--, --S--, --SO.sub.2 --, --PO.sub.2 --, --CO.sub.2 --, --NHCO-- or --NHSO.sub.2 --, wherein L.sub.2 may be orientated in either direction; L.sub.3 is an alkylene group; m is 0 or 1; p is 0 or 1; and X is ##STR2## wherein R' is H or an alkyl or aryl group, with the proviso that where L.sub.2 comprises an ionizable group, X may also be an alkyl group or an aryl group is disclosed. The process comprising the steps of: (a) forming a coarse aqueous slurry of solid particles of said compound; and (b) milling said slurry in the presence of a hydrophobic, photographically inert, liquid second component which has a logP.sub.(calc) greater than about 6.0 for time sufficient to provide particles of the desired average particle size. Solid particle dispersions of the invention exhibit improved raw stock keeping under conditions of elevated temperatures when incorporated in a photographic element.
    • 一种制备式SI的环氧化合物的固体颗粒分散体的方法,其中R是H,烷基或芳基; L1是亚烷基或亚芳基; L 2是-O-,-CO-,-S-,-SO 2 - , - O 2 - , - CO 2 - , - NHCO-或-NHSO 2 - ,其中L2可以沿任一方向取向; L3是亚烷基; m为0或1; p为0或1; 并且X是,其中R'是H或烷基或芳基,条件是其中L2包含可离子化基团,X也可以是烷基或芳基。 该方法包括以下步骤:(a)形成所述化合物的固体颗粒的粗制含水浆料; 和(b)在疏水的,照相惰性的液体第二组分的存在下研磨所述浆料,其中logP(calc)大于约6.0,足以提供所需平均粒径的颗粒。 当结合到照相元件中时,本发明的固体颗粒分散体显示改善的原料保持在高温条件下。
    • 53. 发明授权
    • Color photographic element having improved image stability
    • 具有改进的图像稳定性的彩色照相元件
    • US5597685A
    • 1997-01-28
    • US429269
    • 1995-04-25
    • Krishnan ChariWendell F. Smith, Jr.
    • Krishnan ChariWendell F. Smith, Jr.
    • C07D303/16C07D303/22C07D303/34C07D303/42C07D303/46C07D405/12C07F5/02C07F9/655G03C1/005G03C7/392G03C1/34G03C7/384
    • C07D303/22C07D303/16C07D303/34C07D303/42C07D303/46C07D405/12C07F5/025C07F9/65502G03C1/005G03C7/39268G03C7/39296
    • Color photographic element comprising residual magenta coupler scavenger ionizable epoxy compounds in combination with a specific class of image stabilizers are disclosed. Such elements comprise a support bearing thereon: (a) a photosensitive first layer comprising (i) a silver halide emulsion, (ii) a magenta coupler dispersion, and (iii) an image stabilizer of the following formula STG-A: ##STR1## wherein R.sub.1 represents an alkyl group, a cycloalkyl group, an alkenyl phenyl group, an aryl group, a heterocyclic group, an acyl group, a bridged hydrocarbon group, an alkyl sulfonyl group or an aryl sulfonyl group; R.sub.2 represents a group capable of being substituted on the benzene ring; r represents an integer between 0 and 4; and A represents a group of non metal atoms necessary for the formation of a 5 to 8 membered ring together with the nitrogen atom; and (b) a second layer comprising a dispersion of an epoxy compound of the structural formula SI: ##STR2## wherein R is H, an alkyl group, or an aryl group; L.sub.1 is an alkyl group or an aryl group; L.sub.2 is --O--, --CO--, --S--, --SO.sub.2 --, --PO.sub.2 --, --CO.sub.2 --, --NHCO-- or --NHSO.sub.2 --, wherein L.sub.2 may be orientated in either direction; L.sub.3 is an alkyl group; m is 0 or 1; p is 0 or 1; and X is ##STR3## wherein R' is H or an alkyl or aryl group, with the proviso that where L.sub.2 comprises an ionizable group, X may also be an alkyl group or an aryl group. The photographic elements of the invention exhibit inhibited thermal and photochemical yellowing.
    • 公开了包含残留品红成色剂清除剂可离子化环氧化合物与特定类型的图像稳定剂组合的彩色照相元件。 这样的元件包括其上的支撑轴承:(a)光敏第一层,其包含(i)卤化银乳剂,(ii)品红色成色剂分散体,和(iii)下式STG-A的图像稳定剂: STG-A,其中R1表示烷基,环烷基,烯基苯基,芳基,杂环基,酰基,桥连烃基,烷基磺酰基或芳基磺酰基; R2表示能够在苯环上被取代的基团; r表示0〜4的整数。 A表示与氮原子一起形成5至8元环所必需的一组非金属原子; 和(b)包含结构式SI的环氧化合物的分散体的第二层:其中R是H,烷基或芳基; L1是烷基或芳基; L 2是-O-,-CO-,-S-,-SO 2 - , - O 2 - , - CO 2 - , - NHCO-或-NHSO 2 - ,其中L2可以沿任一方向取向; L3是烷基; m为0或1; p为0或1; 并且X是,其中R'是H或烷基或芳基,条件是其中L 2包含可离子化基团,X也可以是烷基或芳基。 本发明的照相元件表现出抑制的热和光化学黄变。
    • 57. 发明授权
    • Process for selective epoxidation of unsaturated (meth)acrylic compounds
and new bifunctional (meth)acrylates obtained
    • 选择性环氧化不饱和(甲基)丙烯酸类化合物和新型双官能(甲基)丙烯酸酯的方法
    • US5481012A
    • 1996-01-02
    • US335960
    • 1994-11-03
    • Paul CaubereYves FortAgnes Ortar
    • Paul CaubereYves FortAgnes Ortar
    • B01J23/28B01J23/30C07B61/00C07D301/12C07D303/16C07D303/40
    • C07D303/40C07D303/16
    • Process for the epoxidation of an unsaturated (meth)acrylic compound of formula: ##STR1## in which R.sub.1 is chosen from H and C.sub.1 -C.sub.5 -alkyl; R.sub.2 is chosen from H, alkyl and aryl; R.sub.3 is a straight-chain, branched or cyclic alkylene or oxyalkylene radical having from 1 to 12 carbon atoms, it being possible for one of the carbon atoms of R.sub.2, when the latter is an alkyl radical, to be linked to one of the carbon atoms of R.sub.3 to form a ring; and A is chosen from O, S, NH and NR.sub.4, R.sub.4 being a C.sub.1 -C.sub.12 -alkyl group; by the action of hydrogen peroxide on the said unsaturated (meth)acrylic compound, at a temperature of between 10.degree. C. and 50.degree. C., in the presence of at least one catalyst chosen from the alkali metal molybdates and the alkali metal pertungstates and in the presence of at least one phase transfer agent.
    • 式(I)的不饱和(甲基)丙烯酸化合物的环氧化方法,其中R 1选自H和C 1 -C 5 - 烷基; R2选自H,烷基和芳基; R 3是具有1至12个碳原子的直链,支链或环状的亚烷基或氧亚烷基,当其中一个碳原子为烷基时,R2可以与一个碳原子连接 R3的原子形成环; A选自O,S,NH和NR4,R4是C1-C12-烷基; 通过过氧化氢对所述不饱和(甲基)丙烯酸化合物的作用,在10℃至50℃的温度下,在至少一种选自碱金属钼酸盐和碱金属过钨酸盐的催化剂存在下, 并在至少一种相转移剂存在下进行。
    • 58. 发明授权
    • Selective epoxidation of unsaturated (meth)acrylates, new functional
(meth)acrylates, and polymers thereof
    • 不饱和(甲基)丙烯酸酯,新功能(甲基)丙烯酸酯及其聚合物的选择性环氧化
    • US5283360A
    • 1994-02-01
    • US725318
    • 1991-07-08
    • Paul CaubereYves FortAgnes Ortar
    • Paul CaubereYves FortAgnes Ortar
    • B01J23/22B01J23/28B01J23/30B01J27/18B01J31/24C07B35/06C07B41/02C07B61/00C07C67/29C07C69/54C07C233/20C07C327/28C07D301/12C07D301/14C07D303/16C07D303/48C07D317/24C07D317/30C07F7/18C08F20/26C08F20/28C08F20/32C08F30/02C07C69/52
    • C07F7/188C07C67/29C07C69/54C07D303/16C07D317/24C07F7/1852
    • An unsaturated (meth)acrylic compound of formula: ##STR1## (X.dbd.O, S, NH, NR.sup.3 (R.sup.3 =C.sub.1-12 -alkyl) or O--(CH.sub.2).sub.n (where n=1-16 approximately); R.sup.2 =C.sub.2-20 straight-chain or branched alkyl, monocyclic or polycyclic cycloalkyl or heterocycloalkyl, or alkylaryl hydrocarbon chain, comprising an olefinic double bond in the chain, or at the end of the chain in the case of alkyl or alkylaryl, or an exocyclic or endocyclic olefinic double bond in the case of monocyclic or polycyclic cycloalkyl or heterocycloalkyl; and R.sup.1 =H or C.sub.1-5 -alkyl), is reacted at 10.degree.-60.degree. C. with at least one oxidizing compound (hydrogen peroxide) in the presence of at least one catalyst (alkali metal molybdates and tungstates) and in the presence of at least one phase transfer agent and when R.sup.2 =polycyclic cycloalkyl or hetercycloalkyl, an organic peracid or hydrogen peroxide in the presence of at least one heteropolyacid. To open the epoxide function, the epoxide obtained is reacted with a compound chosen from strong inorganic acids, boron trifluoride etherate complexes, acid salts in the presence of the corresponding acid, halides of trialkylsilanes or trialkoxysilanes, and ketones in the presence of cationic resins.
    • (I)(X = O,S,NH,NR 3(R 3 = C 1-12 - 烷基)或O-(CH 2)n)(其中n = 1-16)的不饱和(甲基)丙烯酸化合物 ); R2 = C2-20直链或支链烷基,单环或多环环烷基或杂环烷基或烷基芳基烃链,其在链中包含烯属双键,或在烷基或烷基芳基的情况下在链末端, 在单环或多环环烷基或杂环烷基的情况下为环状或内环烯属双键;且R 1 = H或C 1-5 - 烷基)在10°-60℃下与至少一种氧化化合物(过氧化氢 )在至少一种催化剂(碱金属钼酸盐和钨酸盐)存在下,并且在至少一种相转移剂存在下,并且当R 2 =多环环烷基或杂环烷基时,有机过酸或过氧化氢在至少一种杂多酸 。 为了打开环氧化物官能团,所得环氧化物与选自强无机酸,三氟化硼醚合物络合物,酸盐在相应的酸,三烷基硅烷或三烷氧基硅烷的卤化物,以及阳离子树脂存在下的酮的化合物反应。
    • 59. 发明授权
    • Method and apparatus for synthesis of highly isomerically pure
stereoisomers of glycidol derivatives
    • 合成GLYCIDO衍生物的高纯度异构体纯度的方法和装置
    • US5194637A
    • 1993-03-16
    • US748672
    • 1991-08-22
    • Roger C. Hahn
    • Roger C. Hahn
    • C07C309/71C07D303/16
    • C07D303/16C07C309/71C07C2102/42
    • Methods are provided for producing isomerically enriched camphorsulfonates, and in particular a diastereomerically enriched glycidyl camphorsulfonate by bromide-casylate exchange between an alkyl casylate and the bromide analog of the desired casylate, followed by separation of a higher melting diastereomer by selective recrystallization. There is also shown the production of a desired casylate by reacting a racemic or enantiomerically enriched arenesulfonate with a quaternary casylate. Randomization and recycling of an isomerically enriched casylate is provided by reaction with an achiral bromide analog in the presence of a quaternary salt. Specially adapted apparatus for conducting the randomization reaction is provided. There is also shown a process for producing an alkyl casylate by the reaction of a metal casylate and a quaternary casylate with a trialkyl phosphite in the presence of a slight molar excess of sulfuric acid.
    • 提供了用于通过溴代 - 甲酸酯交换甲磺酸烷基酯和所需的甲磺酸酯的溴化物类似物之间产生异构体富集的樟脑磺酸盐,特别是非对映异构体富集的樟脑磺缩水甘油基缩水甘油酯的方法,然后通过选择性重结晶分离出较高熔点的非对映异构体。 还显示通过使外消旋或对映异构体富集的芳烃磺酸盐与季铵化合物反应制备所需的甲酸酯。 通过在季盐的存在下与非手性溴化物类似物反应来提供异构体富集的甲酸酯的随机化和再循环。 提供了用于进行随机化反应的专用设备。 还显示了在稍微摩尔过量的硫酸存在下,通过金属甲酸酯和季铵化合物与亚磷酸三烷基酯的反应制备烷基酯化的方法。