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41. 发明专利

JPS6429419A CATIONIC PHOTOPOLYMERIZATION INITIATOR 失效
公开(公告)号：JPS6429419A
公开(公告)日：1989-01-31
申请号：JP18409087
申请日：1987-07-23
申请人： WAKO PURE CHEM IND LTD
发明人： HORI MIKIO , KATAOKA SADA , MIYAGAWA TSUTOMU , TAKEUCHI HIDEO
IPC分类号： C08F2/50 , C08G59/00 , C08G59/68 , C08G85/00
摘要： PURPOSE:To obtain the title initiator which has a high molecular absorptivity coefficient and a high polymn. activity and exhibits an excellent fast-curing property in the curing of epoxy resins, by using sulfonium salts of a specified formula as an active ingredient. CONSTITUTION:The title product is a cationic photopolymn. initiator contg. sulfonium salts of the formula as shown [where R is (substd.) aryl; X is a Lewis acid residue which is weakly nucleophilic] or their solvent addition product as an active ingredient. This initiator has a high polymn. activity and exhibits an excellent fast-curing property when it is used in, for example, curing epoxy resins.

42. 发明专利

JPS63264551A PRODUCTION OF CUMINIC ACID 失效
公开(公告)号：JPS63264551A
公开(公告)日：1988-11-01
申请号：JP9916987
申请日：1987-04-22
申请人： WAKO PURE CHEM IND LTD
发明人： MIYAGAWA TSUTOMU , NAWA HIROMI , HIROSE SEIJI
IPC分类号： C07C63/04 , C07C51/285
摘要： PURPOSE:To obtain the titled compound useful as a synthetic intermediate for pharmaceuticals, agricultural chemicals, liquid crystal compound, etc., in high quality without causing the problems of by-product and post-treatment, by oxidizing cuminaldehyde under alkaline condition using hydrogen peroxide as an oxidizing agent. CONSTITUTION:The objective compound of formula II can be produced by oxidizing cuminaldehyde of formula I using hydrogen peroxide as an oxidizing agent under alkaline condition (preferably using sodium hydroxide, potassium hydroxide, etc., to maintain the alkaline state). The above reaction is carried out in a hydrophilic organic solvent such as methanol or dioxane which may contain water. The hydrogen peroxide as an oxidizing agent is usually used as an aqueous solution having a concentration of about 10-40% and the amount of the peroxide is preferably about 1.5-2.5 times mol of the stoichiometric amount based on the cuminaldehyde. The reaction temperature is usually about 60-100 deg.C.

43. 发明专利

JPS6250303A PHOTOPOLYMERIZATION INITIATOR 失效
公开(公告)号：JPS6250303A
公开(公告)日：1987-03-05
申请号：JP19065785
申请日：1985-08-29
申请人： WAKO PURE CHEM IND LTD
发明人： HORI MIKIO , KATAOKA SADA , TANAKA MIKIAKI , MIYAGAWA TSUTOMU , TAKEUCHI HIDEO , TONE HIDEAKI
IPC分类号： C08F2/50 , C07C381/12
摘要： PURPOSE:To obtain a photopolymerization initiator having high polymerizability, freed of problems of toxicity and odor and being excellent in stability, by using a specified sulfonium salt or its solvate as an effective component. CONSTITUTION:A photopolymerization initiator having a sulfonium salt of the formula or its solvate as an effective component. In the formula, R and R are each H or an electron-donating group, R is H or an electron- withdrawing group and X is a Lewis acid residue. Said photopolymerization initiator has a polymerization activity higher than that of benzoin ethyl ether which is a conventional representative photopolymerization initiator. Examples of said electron-donating groups include lower alkoxy, hydroxyl, amino and substituted amino. Examples of said electron-withdrawing groups include halogens, nitro, cyano, carbonyl and carboxyl. Examples of said Lewis acid residues include tetrafluoroboric acid, perchloric acid, antimony hexafluoride and phosphoric acid.

44. 发明专利

JPS61250005A NOVEL MONOMER 失效
公开(公告)号：JPS61250005A
公开(公告)日：1986-11-07
申请号：JP9153785
申请日：1985-04-27
申请人： WAKO PURE CHEM IND LTD
发明人： TANAKA MIKIAKI , MIYAGAWA TSUTOMU , TAKEUCHI HIDEO
IPC分类号： C08F12/00 , C07C25/24 , C08F12/14
摘要： NEW MATERIAL:Fluorine-substituted deuterated styrene derivative of formula I (D is deuterium; m is 1-5; n is integer of 0-4; m+n=5). EXAMPLE:Pentafluoro-pentadeuterated-alpha-methylstyrene (alpha-methylstyrene-F5,d5). USE:Monomer for photoconductive material. Since the compound is free of C-H bond, there is no light absorption in infrared region. The refractive index is lowered moderately by the introduction of C-F bond and the absorption loss caused by C-H bond can be decreased. PREPARATION:alpha-Methylstyrene-F5,d5 of formula IV can be produced e.g. by halogenating pentafluorobenzene (benzene-F5) with a halogen other than F, preparating the Grignard reagent of formula III from the resultant halogenated benzene-F5 of formula II, reacting the reagent with deuterated acetone to obtain the corresponding benzyl-type carbinol and eliminating the tert-OH substituted to the benzyl group.

45. 发明专利

JPS6128521A Novel polymer and its production 失效
标题翻译：新型聚合物及其生产
公开(公告)号：JPS6128521A
公开(公告)日：1986-02-08
申请号：JP14035684
申请日：1984-07-06
申请人： Takeda Chem Ind Ltd , Wako Pure Chem Ind Ltd
发明人： TANAKA MIKIAKI , OGAWA TAIRYO , MIYAGAWA TSUTOMU , WATANABE TOSHIO
IPC分类号： C08G63/00 , A61K47/34 , C08G63/06 , C08G63/82
摘要： PURPOSE: To obtain a novel polymer having a specified weight-average MW and a specified degree of dispersion and usable chiefly as a pharmaceutical base for medicines, by reacting lactic and/or glycolic acid in the presence or absence of an inorganic solid acid catalyst.
CONSTITUTION: Lactic and/or glycolic acid are mixed together at an arbitrary ratio usually without using any solvent and directly polycondensed in the absence of any catalyst, i.e., without using any polymerization catalyst, or in the presence of an inorganic solid acid catalyst (e.g., acid clay), while the water formed is being removed by heating in vacuum. The reaction temperature and time are 100W150°C and 350W30mmHg, respectively. The water is removed while the temperature and the degree of vacuum are increased stepwise over a period of 2hr and then the reaction mixuture is polycondensed by dehydration at 150W 200°C/10W1mmHg for 10hr or longer. In this way, a polymer or copolymer having a weight-average MW ≥about 5,000 and a degree of dispersion of about 1.5W 2 can be obtained.
COPYRIGHT: (C)1986,JPO&Japio
摘要翻译：目的：为了获得具有特定重均分子量和特定分散度的新型聚合物，主要用作药物的药用基质，通过乳酸和/或乙醇酸在无机固体酸催化剂存在或不存在下反应。构成：乳酸和/或乙醇酸通常以任意比例混合在一起而不使用任何溶剂，并在没有任何催化剂的情况下直接缩聚，即不使用任何聚合催化剂，或在无机固体酸催化剂存在下（例如，酸性粘土），而形成的水通过在真空中加热而除去。反应温度和时间分别为100-150℃和350-30mm.Hg。除去水，同时在2小时内逐步增加温度和真空度，然后将反应混合物在150-200℃/ 10-1mm.Hg下脱水缩聚10小时以上。以这种方式，可以获得重均分子量>约5,000，分散度约1.5-2的聚合物或共聚物。

46. 发明专利

JPS58195806A Manufacture of plastic optical fiber with small loss 失效
标题翻译：具有小损失的塑料光纤的制造
公开(公告)号：JPS58195806A
公开(公告)日：1983-11-15
申请号：JP7888182
申请日：1982-05-11
申请人： Nippon Telegr & Teleph Corp , Wako Pure Chem Ind Ltd
发明人： KAINOU TOSHIKUNI , JINGUUJI KANAME , NARA SHIGEO , TANAKA MIKIAKI , MIYAGAWA TSUTOMU , NAWA HIROMI , TAKEUCHI HIDEO
IPC分类号： G02B1/04 , B29D11/00 , C08F4/04 , C08F20/14 , G02B6/00
CPC分类号： B29D11/00663
摘要： PURPOSE:To obtain an optical fiber with small loss and superior light transmitting characteristics in the visible light region, by adding a chain transfer agent and an azo compound to a methyl methacrylate (MMA) monomer under tightly sealed conditions in the absence of oxygen, polymerizing the monomer, and melt-spinning the resulting MMA polymer to form a core fiber. CONSTITUTION:An MMA-base polymer is used as a core, and a sheath of a synthetic polymer having a lower refractive index than the core is formed around the core to manufacture a plastic optical fiber. At this time, an MMA monomer is purified in a tightly sealed system, and to the monomer in the absence of oxygen are added a chain transfer agent and an azo compound represented by the formula (where each of R1-R3 is straight or branched chain 1-5C alkyl or cycloalkyl, and the total number of C of R1-R3 is
摘要翻译：目的：为了获得可见光区域损耗小，透光性能优异的光纤，通过在不存在氧的情况下，在密闭条件下向甲基丙烯酸甲酯（MMA）单体中添加链转移剂和偶氮化合物，聚合并将所得MMA聚合物熔融纺丝以形成芯纤维。构成：使用MMA基聚合物作为芯，并且在芯周围形成具有比芯低的折射率的合成聚合物的护套以制造塑料光纤。此时，MMA单体在紧密密封的系统中纯化，在不存在氧的情况下向单体加入链转移剂和由式（其中R 1 -R 3为直链或支链的每一个） 1-5C烷基或环烷基，并且R1-R3的总数为<= 7）为聚合物。引发剂在密封条件下。将得到的芯聚合物在密封状态下熔融纺丝以形成芯纤维。

47. 发明专利

JPS58192857A Preparation of mixture from azo compound 失效
标题翻译：从AZO化合物制备混合物
公开(公告)号：JPS58192857A
公开(公告)日：1983-11-10
申请号：JP6827083
申请日：1983-04-20
申请人： Wako Pure Chem Ind Ltd
发明人： YAMASHITA KAZUHIKO , MIYAGAWA TSUTOMU , SUGANO MASAHIKO , MINAMII NOBUAKI , NAGAOKA JIYOUJI
IPC分类号： C07C255/42 , C07C67/00 , C07C253/00 , C07C255/65
摘要： PURPOSE: To obtain the titled compound useful as a polymerization initiator having various decomposition rate constants by a highly industrially valuable method, by oxidizing a hydrazo compound containing a novel asymmetric hydrazo compound.
CONSTITUTION: A mixture of hydrazo compounds containing an asymmetric hydrazo compound of formula I (R
1 , R
2 , R
3 and R
4 are alkyl, cycloalkyl, phenyl, etc.; R
1 and R
2 and/or R
3 and R
4 may form a ring except a symmetric compound having the same group consisting of R
1 and R
2 as the group consisting of R
3 and R
4 ) is oxidized with an oxidizing agent, e.g. halogen, or with oxygen in the presence of a metallic oxide as a catalyst in an aqueous medium or organic solvent system to give the aimed compound of formula II.
EFFECT: The continuous polymerization can be carried out, and various polymerization temperatures can be selected for monomers. Thus, a polymer having new conventionally unobtainable properties is obtained.
COPYRIGHT: (C)1983,JPO&Japio
摘要翻译：目的：通过高度工业上有价值的方法获得用作具有各种分解速率常数的聚合引发剂的标题化合物，通过氧化含有新的不对称氢化合物的水解化合物。构成：含有式I的不对称氢化合物（R 1，R 2，R 3和R 4）的氢化合物的混合物是烷基，环烷基，苯基等; R 1和R 2 >和/或R 3和R 4可以形成环，除了具有与作为R 3和R 4的R 1和R 2相同的基团的对称化合物，）用氧化剂氧化，例如卤素或氧气在金属氧化物作为催化剂存在下在水性介质或有机溶剂体系中反应，得到目的化合物II。效果：可以进行连续聚合，可以选择单体的各种聚合温度。因此，获得具有新的常规无法获得的性质的聚合物。

48. 发明专利

JPS58177969A Preparation of piperidinoalkanol and its acid addition salt 失效
标题翻译：哌啶醇及其酸添加盐的制备
公开(公告)号：JPS58177969A
公开(公告)日：1983-10-18
申请号：JP6133782
申请日：1982-04-13
申请人： Wako Pure Chem Ind Ltd
发明人： TANAKA MIKIAKI , MIYAGAWA TSUTOMU , NAKADA TAKASHI
IPC分类号： C07D211/14 , C07D213/30
摘要： PURPOSE: To obtain the titled compound in high yield, by hydrogenating a novel quaternary ammonium salt as a raw material obtained from 4-(α-acetoxybenzyl) pyridine and a specific compound in the presence of an organic acid, its alkali metal salt and a catalyst.
CONSTITUTION: 4-(α-Acetoxybenzyl)pyridine is reacted with a compound shown by the formula I (X is halogen) in a solvent to give a novel quaternary ammonium salt shown by the formula II, which is hydrogenated in the presence of a hydrogenating catalyst such as Pd/Cd, etc., an organic acid and its alkaline (earth)metal salt in a solvent at 40W60°C for 1W10hr at atmospheric pressure W50kg/cm
2 hydrogen pressure under weakly acidic conditions, to give the desired compound shown by the formula III. Acetic acid, formic acid, propionic acid, etc. and their Na, K, Li, Mg salts are used as the organic acid and its alkaline(earth)metal salts.
EFFECT: No corrosion of a device during reaction.
USE: An improver for cerebral circulation metabolism.
COPYRIGHT: (C)1983,JPO&Japio
摘要翻译：目的：为了获得高收率的标题化合物，通过在有机酸存在下氢化新的季铵盐作为由4-（α-乙酰氧基苄基）吡啶和特定化合物得到的原料，其碱金属盐和催化剂。构成：将4-（α-乙酰氧基苄基）吡啶与式I所示化合物（X为卤素）在溶剂中反应，得到式II所示的新型季铵盐，其在氢化存在下氢化催化剂如Pd / Cd等，有机酸及其碱土金属盐在溶剂中在40-60℃下在大气压力-50kg / cm 2氢压下在弱酸性下进行1-10小时条件，得到式III所示的所需化合物。乙酸，甲酸，丙酸等及其Na，K，Li，Mg盐用作有机酸及其碱土金属盐。影响：反应期间设备不会腐蚀。用途：脑循环代谢改善剂。

49. 发明专利

JPS5798260A QUATERNARY AMMONIUM SALT AND ITS PREPARATION 失效
公开(公告)号：JPS5798260A
公开(公告)日：1982-06-18
申请号：JP17411680
申请日：1980-12-10
申请人： WAKO PURE CHEM IND LTD
发明人： TANAKA MIKIAKI , MIYAGAWA TSUTOMU , NAKADA TAKASHI
IPC分类号： C07D211/14 , C07D213/50
摘要： NEW MATERIAL:A quaternary ammonium salt shown by the formulaI[R is aryl; R' is H or a group (e.g., benzyl, acetyl, propionyl, tosyl, etc.) to be replaced by H; X is halogen]. EXAMPLE:1-[1-(4-Hydroxyphenyl,carbonyl)-ethyl]-4-benzoylpyridinum bromide. USE:An intermediate for a piperidinoalkanol(improver for cerebral circulatory metabolism) shown by the formula II. The compound shown by the formula II can be obtained easily in high yield. PROCESS:A 4-benzoylpyridine shown by the formula III is reacted with a compound[e.g., 1-(4-hydroxyphenyl)-2-bromopropane-1-one, etc.]shown by the formula IV, to give a compound shown by the formulaI.

50. 发明专利

JPS55161877A LOW FREEZING POINT COMPOSITION 失效
公开(公告)号：JPS55161877A
公开(公告)日：1980-12-16
申请号：JP6832579
申请日：1979-06-01
申请人： WAKO PURE CHEM IND LTD
发明人： NAGAOKA JIYOUJI , TANAKA MIKIAKI , MIYAGAWA TSUTOMU , YAMAGUCHI OSAMU , INOUE KATSUSUMI
IPC分类号： C09K3/00
摘要： PURPOSE:A thixotropic, semisolid, low freezing point composition which protects driving members from freezing due to coldness, comprising, as main components, water, an alcohol, polyacrylic acid or a salt thereof. CONSTITUTION:A low freezing point composition prepared by thickening a mixture of (A) water and (B) at least one alcohol with (C) polyacrylic acid or a salt thereof. Examples of the component (B) include methanol, ethanol and ethylene glycol. The weight ratio of (A) to (B) is preferably 5:1-1:1. With respect to the amount of (C), usually, 0.1-3wt% is satisfactory to obtain a desirable effect.

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