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11. 发明专利

JPS5661350A PREPARATION OF CYSTEAMINE HYDROCHLORIDE 失效
公开(公告)号：JPS5661350A
公开(公告)日：1981-05-26
申请号：JP13845479
申请日：1979-10-25
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , YONEZAWA TAIZOU
IPC分类号： C07C319/02 , C07C67/00 , C07C313/00 , C07C323/25
摘要： PURPOSE:To prepare the titled compound useful as a synthetic intermediate of organic chemicals, pesticides, and pharmaceuticals, in a short step, by reacting an aqueous solution of 2-chloroethylamine hydrochloride with an alkali hydrosulfide or thiourea at pH5-13. CONSTITUTION:The objective compound is prepared by mixing a 5-60% aqueous solution of 2-chloroethylamine hydrochloride of pH5-13 with an alkali hydrosulfide (e.g. sodium hydrosulfide, potassium hydrosulfide and ammonium hydrosulfide) or thiourea, and heating the mixture, pref. at 30-70 deg.C under stirring. 2-Chloroethylamine is stable even under alkaline conditions within pH5-13, and there is little polymerization and tar formation of the amine by heating.

12. 发明专利

JPS5612336A PREPARATION OF ALPHAABROMOCARBOXYLIC ACID HALIDE 失效
公开(公告)号：JPS5612336A
公开(公告)日：1981-02-06
申请号：JP8794679
申请日：1979-07-10
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , YONEZAWA TAIZOU , KOUNE NOBUHIRO
IPC分类号： C07C53/50 , B01J27/00 , B01J27/02 , B01J27/10 , C07B61/00 , C07C51/00 , C07C51/60 , C07C67/00
摘要： PURPOSE:To obtain the titled compound, an intermediate of pharmaceuticals and pesticides, in high yield with easy isolation and with little formation of side products, by the reaction of an alpha-bromocarboxylic acid with a halogenating agent using sulfuric acid or a Lewis acid as a catalyst. CONSTITUTION:The titled compound is obtained by the reaction of an alpha-bromocarboxylic acid of formula (R is methyl, ethyl, or isopropyl) with a halogenating agent, preferably thionyl chloride, preferably at 30-100 deg.C in the presence of sulfuric acid and/or a Lewis acid, e.g. AlCl3, as a catalyst. The amount of the catalyst is ca. 0.01-1mol% of the starting material alpha-bromocarboxylic acid, and that of the thionyl chloride as halogenating agent is preferably 1.0-1.5mol. The starting material of formula is obtained, e.g. by reacting isovaleric acid with bromine at 70-80 deg.C in the presence of PCl3 catalyst.

13. 发明专利

JPS54106422A PREPARATION OF BROMOISOVALEROYL CHLORIDE 失效
公开(公告)号：JPS54106422A
公开(公告)日：1979-08-21
申请号：JP1320678
申请日：1978-02-07
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , YONEZAWA TAIZOU
IPC分类号： C07C53/50 , C07C51/00 , C07C51/58 , C07C67/00
摘要： PURPOSE:To prepare the title compound useful as a raw material of 2-bromo-3- methylbutyryl urea which is a known narcotic and analgesic agent, economically without emitting ill odor, by brominating isovaleric acid with bromine, and without separating the product, converting the brominated compound to the corresponding acid chloride. CONSTITUTION:alpha-Bromoisovaleroyl chloride is prepared by (1) brominating the alpha-position of isovaleric acid (1 mole) with bromine (1.0-1.5 moles) at 60-90 deg.C, and without isolating the product, (2) converting the brominated compound to the corresponding acid chloride by reacting with thionyl chloride (1.0-1.5 moles) or phosphorus trichloride (0.3-1.5 moles) in the presence of pyridine, etc.

14. 发明专利

JPS63166861A PRODUCTION OF 1,4-BENZENETHIOL 失效
公开(公告)号：JPS63166861A
公开(公告)日：1988-07-11
申请号：JP31570486
申请日：1986-12-27
申请人： SEITETSU KAGAKU CO LTD
发明人： TAKAHASHI MASAHIDE , KAWAMURA MASAO , KATO KUNIOKI , SUZUKI MICHIO , MASUDA YOSHIHIDE
IPC分类号： B01J27/06 , B01J27/00 , B01J27/138 , C07B61/00 , C07C67/00 , C07C313/00 , C07C319/02 , C07C321/26
摘要： PURPOSE:To safely obtain 1,4-benzenethiol in a simple process, by reacting thiophenol or diphenyl disulfide with sulfur chloride in the presence of a catalyst and reducing the resultant product. CONSTITUTION:Thiophenol or diphenyl disulfide which is an oxidation product thereof is reacted with sulfur chloride in the presence of iodine or a Friedel- Crafts reaction catalyst, e.g. zinc chloride, in a solvent, e.g. chloroform, etc., at room temperature - boiling point of the solvent and the resultant product is then reduced with zinc and hydrochloric acid to afford the aimed substance. The reaction is carried out by using the Friedel-Crafts catalyst and iodine in a molar amount of 0.05-2 times based on the thiophenol. The obtained substance is useful as a material for highly functional engineering plastics having excellent heat and chemical resistance or raw material for producing sulfur- containing polymers useful as a material for organic glass having a high refractive index utilizing high atomic refraction of the sulfur.

15. 发明专利

JPS62246932A PRODUCTION OF POLYARYLENE SULFIDE 失效
公开(公告)号：JPS62246932A
公开(公告)日：1987-10-28
申请号：JP9039086
申请日：1986-04-18
申请人： SEITETSU KAGAKU CO LTD
发明人： TAKAHASHI MASAHIDE , KAWAMURA MASAO , KATO KUNIOKI , SUZUKI MICHIO
IPC分类号： C08G75/02 , C08G75/0213 , C08G75/06
摘要： PURPOSE:To enable the reaction to proceed at a temperature lower than that in a conventional process and to improve yields, by reacting a thiphenol with sulfuryl chloride in a solvent in the presence of a Friedel-Crafts reaction catalyst. CONSTITUTION:A thiophenol of formula I (wherein R1, R2, R3 and R4, which are independent of each other and may be the same, are H, halogens or 1-3C alkyls) is reacted with sulfuryl chloride in a solvent in the presence of a Friedel- Crafts reaction catalyst. As the Friedel-Crafts reaction catalyst, aluminum chloride is usually used. Examples of the reaction solvents which can be mentioned include benzene, thiophenol, diphenyl sulfide and a mixture of one of them with a halogenated hydrocarbon. The reaction temperature is preferably 20-80 deg.C.

16. 发明专利

JPS6150934B2 失效
公开(公告)号：JPS6150934B2
公开(公告)日：1986-11-06
申请号：JP10645483
申请日：1983-06-13
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , HATA HIROYUKI , MORISHITA TSUYOSHI
IPC分类号： C07C59/185 , C07C51/00 , C07C51/09 , C07C67/00

17. 发明专利

JPS5953259B2 失效
公开(公告)号：JPS5953259B2
公开(公告)日：1984-12-24
申请号：JP3781782
申请日：1982-03-09
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , HAMAYA KAZUHIRO
IPC分类号： C07D213/64 , B01J31/02 , B01J31/06 , C07B61/00

18. 发明专利

JPS58198480A Preparation of ketopantolactone 失效
标题翻译： Ketopantolactone的制备
公开(公告)号：JPS58198480A
公开(公告)日：1983-11-18
申请号：JP8206182
申请日：1982-05-14
申请人： Seitetsu Kagaku Co Ltd
发明人： KAWAMURA MASAO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE , HATA HIROYUKI
IPC分类号： C07D307/60
摘要： PURPOSE: To obtain economically the titled substance useful as a raw material for pantothenic acid, a major raw material for synthesis of vitamins, by condensing isobutylaldehyde with an oxalic ester, reducing the reaction product in the presence of an alkali.
CONSTITUTION: Isobutylaldehyde shown by the formula I is condensed with an oxalic ester shown by the formula II (R and R' in the formula are 1W5C alkyl, n=5) in the presence of a base (e.g., sodium methalate, caustic soda) as a catalyst at 10W60°C to give α-oxoβ-formylisovaleric acid shown by the formula III, which is reacted with glyoxylic acid or formaldehyde under alkali conditions (pH is kept at ≥12) at 0W100°C, and the system is acidified with an aqueous solution of hydrochloric acid, sulfuric acid, etc., to give the titled substance shown by the formula IV. In the second process, after the reaction of the first process is over, the alkali and glyoxylic acid, etc. are added to the reaction product, and the pH and the temperature are adjusted, so that the process may be carried out successively without isolating the condensation product.
COPYRIGHT: (C)1983,JPO&Japio
摘要翻译：目的：经济地获得用作泛酸原料的标题物质，泛酸是通过将异丁醛与草酸酯缩合来还原合成维生素的主要原料，在碱存在下还原反应产物。构成：式I所示的异丁醛与式II所示的草酸酯（式中的R和R'在1-5C烷基，n = 5）在碱（例如甲酸钠，苛性碱）存在下缩合苏打）作为催化剂，在10-60℃下，得到式III所示的α-氧代 - 甲酰基异戊酸，其在碱性条件下（pH保持在> = 12）下与乙醛酸或甲醛反应，在0-100℃ 将该体系用盐酸，硫酸等的水溶液酸化，得到式Ⅳ所示的标题物质。在第二工序中，第一工序的反应结束后，将碱金属和乙醛酸等添加到反应产物中，调节pH和温度，使得可以连续进行，而不进行分离缩合产物。

19. 发明专利

JPS5564583A PREPARATION OF THIOPHENECARBONYL CHLORIDE 失效
公开(公告)号：JPS5564583A
公开(公告)日：1980-05-15
申请号：JP13812278
申请日：1978-11-08
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , NISHI TADAAKI , AKUTSU SEIICHI , KATOU KUNIKIYO , TAKAHASHI MASAHIDE , YONEZAWA TAIZOU , KANAZAWA TADASHI
IPC分类号： C07D333/38 , C07D333/24
摘要： PURPOSE:To obtain the title substance useful as an intermediate for medicines, and pesticides in high yield, by reacting thiophene aldehyde with chlorine in the presence of a radical initiator or with ultraviolet irradiation in the absence of a catalyst. CONSTITUTION:Thiophene aldehyde (T) of formula I is reacted with chlorine (C) in the presence of 0.05-10wt% based on (T) of a radical initiator or by ultraviolet irradiation in the absence of a catalyst at room temperature to 200 deg.C at a molar ratio of (C) to (T) of 0.7-10 if necessary in a solvent, e.g. carbon tetrachloride, benzene, or monochlorobenzene. An azo compound inorganic peroxide, e.g. potassium persulfate, or an organic peroxide, e.g. benzoyl peroxide, may be used as the initiator.

20. 发明专利

JPS5419964A PREPARATION OF THIOPHENEESUBSTITUTED FATTY ACID HALODE 失效
公开(公告)号：JPS5419964A
公开(公告)日：1979-02-15
申请号：JP8310677
申请日：1977-07-11
申请人： SEITETSU KAGAKU CO LTD
发明人： KAWAMURA MASAO , TSUCHIYA HIROO , AKUTSU SEIICHI , TAKAHASHI MASAHIDE
IPC分类号： C07D333/24 , C07D333/16 , C07D333/38
摘要： PURPOSE:In the preparation of title compound by halogenation of a thiophenesubstituted fatty acid with a halogenating agent, the water in the fatty acid is removed by using an organic solvent in the form of an azeotropic mixture, thus simplifying the process and improving the yield.

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