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1. 发明专利

JPS60116674A PRODUCTION OF 5-AMINOISOXAZOLE 失效
公开(公告)号：JPS60116674A
公开(公告)日：1985-06-24
申请号：JP22333583
申请日：1983-11-29
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , ASADA HIDEKI , FUJIWARA YOSHIMI
IPC分类号： C07D261/14
摘要： PURPOSE:To produce 5-aminoisoxazole useful as a raw material of phamaceuticals and agricultrual chemicals, etc, from a raw material available easily at a low cost, in high yield, without using a catalyst, by reacting 3-alkoxyacrylonitrile with hydroxylamine. CONSTITUTION:5-Aminoisoxazole can be produced economically in an industrial scale, by reacting (A) 1mol of 3-alkoxyacrylonitrile of formula ROCH=CHCN (R is 1-8C alkyl which may have substituent group inert to the reaction, e.g. alkoxy, halogen, etc.) with (B) 0.1-10mol, preferably 0.5-5mol of hydroxylamine, in (C) an inert good solvent of the raw materials usually at 10-150 deg.C for 0.5-10hr. The hydroxylamine may be used as the amine form, however, it is usually used as a salt such as sulfate, hydrochloride, nitrate, phosphate, acetate, etc.

2. 发明专利

JPS565429A PREPARATION OF ACETAL 失效
公开(公告)号：JPS565429A
公开(公告)日：1981-01-20
申请号：JP7968979
申请日：1979-06-26
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , IWAYAMA KIYOSHI , ABE TAKAAKI , MATSUNAGA HIROBUMI
IPC分类号： C07C43/303 , B01J23/00 , B01J23/44 , B01J27/00 , B01J27/24 , C07B61/00 , C07C41/00 , C07C41/50 , C07C41/54 , C07C67/00
摘要： PURPOSE:To obtain the titled compound useful as a raw material of agricultural chemicals, in high yield without using a special apparatus and complicated operations, by using a nitrous acid ester as a cocatalyst in the reaction of an alpha-olefin, an alcohol and oxygen in the presence of a palladium metal catalyst. CONSTITUTION:The titled compound is obtained by the catalytic reaction of an alpha- olefin, an alcohol and oxygen, usually at 20-150 deg.C under atmospheric or positive pressure, using palladium metal or its salts as a catalyst and a nitrous acid ester as a cocatalyst. Said catalyst is favorably used in the range of 0.001-5g, reduced to palladium metal, to 100ml of the raw material alcohols, and the co-catalyst is favorably used in the range of at least 0.05 times, preferably 0.1-5 times the volume of the raw material alcohol. Methyl nitrite, butyl nitrite, decyl nitrite, etc. are useful as the nitrous acid ester.

3. 发明专利

JPS5217415A PROCESS FOR PREPARATION OF OXALIC ACID DIESTER 失效
公开(公告)号：JPS5217415A
公开(公告)日：1977-02-09
申请号：JP9210275
申请日：1975-07-30
申请人： UBE INDUSTRIES
发明人： EGUCHI KATSUIKI , UCHIUMI SHINICHIROU , KIYOMOTO TOSHIO , TAKAHASHI MITSUO
IPC分类号： C07C69/36 , B01J23/00 , B01J23/38 , B01J23/42 , B01J23/44 , B01J23/46 , B01J31/00 , B01J31/02 , C07B61/00 , C07C67/36
摘要： PURPOSE:Oxalic acid diester, useful as analytical reagents, solvents, raw materials of oxamide or orotic acid, is prepared in high yield and high selectively by the reaction of an aliphatic alcohol with carbon monoxide and oxygen under pressure in the presence of a catalyst, a reaction accelerator and a side reaction inhibitor such as nitrobenzene.

4. 发明专利

JPS60116659A PRODUCTION OF ALPHA-(3,4,5-TRIMETHOXYBENZYL)-BETA,BETA- DIALKOXYPROPIONITRILE 失效
公开(公告)号：JPS60116659A
公开(公告)日：1985-06-24
申请号：JP22333883
申请日：1983-11-29
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , ASADA HIDEKI , UMETSU TAKASHI
IPC分类号： C07B61/00 , B01J31/00 , B01J31/02 , B01J31/28 , C07C67/00 , C07C253/00 , C07C253/30 , C07C255/37
摘要： PURPOSE:To produce the titled compound useful as a synthetic intermediate of agricultural chemicals and phamaceuticals, in high yield, by reducing alpha-(3,4,5-trimethoxybenzylidene)-beta,beta-dialkoxypropionitrile with hydrogen in the presence of palladium metal and an amine. CONSTITUTION:The objective compound of formula II can be produced by reducing an alpha-(3,4,5-trimethoxybenzylindene)-beta,beta-dialkoxypropionitrile of formula I (R is lower alyl) with hydrogen in the presence of palladium metal catalyst (e.g. palladium supported by activate carbon) and an amine (e.g. dimethylamine, triethylamine, etc.) in a solvent such as water, methanol, ethanol, etc. at 20- 100 deg.C under atmospheric or positive pressure.

5. 发明专利

JPS60116650A PRODUCTION OF HALOGENATED VINYL ETHER 失效
公开(公告)号：JPS60116650A
公开(公告)日：1985-06-24
申请号：JP22333783
申请日：1983-11-29
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , ASADA HIDEKI , UMETSU TAKASHI
IPC分类号： C07C69/734 , C07C67/00 , C07C67/307 , C07C67/317 , C07C253/00 , C07C253/30 , C07C255/13 , C07C255/15
摘要： PURPOSE:To produce the titled compound useful as a raw material of pharmaceuticals, agricultural chemicals, etc., easily, by using an inexpensively and easily available vinyl ether as a raw material, reacting the vinyl ether with a halogen, and treating the reaction product with a base. CONSTITUTION:A vinyl ether is made to react with a halogen (preferably chlorine or bromine) at =0.5mol, preferably 1-10mol per 1mol of the vinyl ether. The vinyl ether used as a raw material is a compound represented by the formula R O CH=CH-Y (R is methyl, ethyl, etc.; Y is CN, etc.).

6. 发明专利

JPS60115567A PRODUCTION OF 3-AMINOISOXAZOLE 失效
公开(公告)号：JPS60115567A
公开(公告)日：1985-06-22
申请号：JP22079883
申请日：1983-11-25
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , ASADA HIDEKI
IPC分类号： C07D261/14 , C07D261/04
摘要： PURPOSE:To obtain the titled compound useful as a raw material for mdeicines and agricultural chemicals, etc. in high yield using inexpensive and easily available raw materials, by reacting a 3-alkoxyacrylonitrile with hydroxylamine in the presence of an alkali metal hydroxide. CONSTITUTION:A 3-alkoxyacrylonitrile of the formula ROCH=CHCN [R is 1-8C alkyl (which may be substituted by alkoxy or halogen, etc.)] is reacted with 0.1-10mol, based on 1mol 3-alkoxyacrylonitrile, hydroxylamine in a solvent, e.g. water, in the presence of an alkali metal hydroxide, e.g. NaOH, at 10-150 deg.C for 0.5-10hr to afford the aimed compound. The hydroxylamine is used in the form of a salt, e.g. sulfate, hydrochloride, nitrate, phosphate, acetate or toluenesulfonate, etc. The amount of the alkali metal hydroxide to be used is 1-10mol based on 1mol hydroxylamine salt. If the amount of the alkali metal hydroxide to be used is larger than 1.5mol, the aimed compound is directly obtained.

7. 发明专利

JPS5821636A PREPARATION OF ACETAL 失效
公开(公告)号：JPS5821636A
公开(公告)日：1983-02-08
申请号：JP11841081
申请日：1981-07-30
申请人： UBE INDUSTRIES
发明人： MATSUTAME CHIKANOBU , UCHIUMI SHINICHIROU , IWAYAMA AKIRA , UMETSU TAKASHI
IPC分类号： C07C69/66 , B01J23/00 , B01J23/74 , B01J27/00 , B01J27/08 , B01J27/24 , B01J31/00 , B01J31/04 , C07B61/00 , C07C41/00 , C07C41/54 , C07C43/30 , C07C67/00 , C07C67/31 , C07C253/00 , C07C255/13
摘要： PURPOSE:In reacting an olefin with an alcohol and an ester of nitrous acid, to obtain the titled substance useful as a raw material for synthesizing agricultural chemicals, etc. by a simple operation in high yield, by contacting them in a gaseous phase in the presence of both a platinum group metal and an iron compound. CONSTITUTION:An olefin such as ethylene, propylene, etc. is brought into contact with an alcohol and an ester of nitrous acid using a platinum group metal such as palladium, platinum, etc. or their hydrochlorides as a catalyst and an iron compound as a cocatalyst in a gaseous phase, to give an acetal. The reaction is carried out usually in a temperature range of 50-200 deg.C at normal pressure or under pressure, for example, at (gauge). FeCl2, FeCl3.6H2O, FeBr3, etc. are useful as the iron compound, and its amount used is an amount to give an atom ratio of iron to the platinum group metal or 0.1-10, preferably 0.5-5.

8. 发明专利

JPS57203051A PREPARATION OF MALONONITRILE 失效
公开(公告)号：JPS57203051A
公开(公告)日：1982-12-13
申请号：JP8747081
申请日：1981-06-09
申请人： UBE INDUSTRIES
发明人： MATSUTAME CHIKANOBU , UCHIUMI SHINICHIROU , TAKAHASHI MITSUO , ASADA HIDEKI , KURAHASHI MASARU
IPC分类号： C07C255/04 , C07C67/00 , C07C253/00
摘要： PURPOSE:To prepare the titled compound useful as a raw material of vitamin B1, in high yield and selectivity, economically in an industrial scale, by treating cyanoacetaldehyde acetal in an aqueous solution of an acid, and reacting with hydroxylamine-o-sulfonic acid. CONSTITUTION:The cyanoacetaldehyde acetal of formula (R is H, alkyl, etc.; R' is alkyl, etc.; the H in the alkyl groups R and R' may be substituted with halogen, etc.) is treated in an acidic aqueous solution (e.g. sulfuric acid solution) at 20-100 deg.C, and made to react with hydroxyalmine-o-sulfonic acid at 0- 100 deg.C to obtain the objective compound. EFFECT:Since the reaction process is simplified, the safety of the raw material is high and the corrosion of the apparauts to inhibited compared with the conventional process, the treatment of the waste water and waste liquid can be simplified, and the necessity of using a reaction apparatus made of a particular material can be eliminated.

9. 发明专利

JPS56155008A PREPARATION OF HYDROXYAMINE-O-SULFONIC ACID 失效
公开(公告)号：JPS56155008A
公开(公告)日：1981-12-01
申请号：JP5350680
申请日：1980-04-24
申请人： UBE INDUSTRIES
发明人： UCHIUMI SHINICHIROU , TAKAHASHI MITSUO
IPC分类号： C01B21/093
摘要： PURPOSE:To prepare high-purity hydroxylamine-O-sulfonic acid in high yield easily, by bringing a mineral acid salt of hydroxylamine into contact with sulfur trioxide gas so that they are reacted in solid-vapor state. CONSTITUTION:Sulfur trioxide gas (may be diluted with an inert gas, e.g., nitrogen, methane, etc.) is brought into contact with a solid mineral acid salt of hydroxylamine (preferably a sulfate having a particle size about 40-250 mesh) at about 20-100 deg.C for about 5-10hr. The mineral acid liberated by the reaction is attached to the reaction product, but it can be removed easily by washing the reaction product with an ether or acetic ester.

10. 发明专利

JPS54100312A PREPARATION OF OXALIC DIESTERS 失效
公开(公告)号：JPS54100312A
公开(公告)日：1979-08-08
申请号：JP615078
申请日：1978-01-25
申请人： UBE INDUSTRIES
发明人： NISHIMURA KENJI , FUJII KOUZOU , NISHIHIRA KEIGO , MATSUDA MASAOKI , UCHIUMI SHINICHIROU
IPC分类号： C07C69/36 , B01J23/00 , C07C67/36 , C07C68/00
摘要： PURPOSE:To prepare the title compounds which are raw materials of oxalic acid, oxamide, etc., on an industrial scale, by the vapor-phase catalytic reaction of CO and nitrous ester, or CO, alcohol and nitrogen oxide or its hydrate in the presence of a long-life catalyst comprising supported Pd or its salt. CONSTITUTION:Oxalic diesters of formular II are prepared by the vapor-phase catalytic reaction of CO and esters of formula I (R is alkyl or cycloalkyl) derived from 1-8C saturated monohydric aliphatic or alicyclic alcohols and nitrous acid, or CO, alcohols and nitrogen oxides, such as NO, NO2, N2O3 and N2O4, or hydrates of nitrogen oxides, such as nitric acid and nitrous acid, in the presence of a solid catalyst supporting Pd metal or its mitrate, sulfate, phosphate, etc. on alumina, silica, etc., at 50-200 deg.C. EFFECT:Compared with the liquid phase reaction, the desired compounds are obtained in high selectivity and high space time yield even under normal (low) pressure. There is no dissolution loss of Pd. USE:Raw materials for syntheses of glycols, intermediates of dyes, medicines, etc.

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