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1. 发明专利

JPS61137873A Production of n,n-pentamethylenethiolcarbamic acid alkali metal salt 失效
标题翻译：生产N，N-戊酸乙酯酸性碱金属盐
公开(公告)号：JPS61137873A
公开(公告)日：1986-06-25
申请号：JP25931184
申请日：1984-12-10
申请人： Mitsubishi Petrochem Co Ltd
发明人： AYUSAWA TADASHI , IWANE HIROSHI , KUJIRA KATSUFUMI , KAWAHARA TAKAYUKI , TSUKAMOTO SEIICHI
IPC分类号： C07D295/02 , C07D295/20
摘要： PURPOSE: To obtain an aqueous layer containing the titled substance, by reacting an alkali metal hydroxide to an organic solvent solution of an N,N- pentamethylenethiolcarbamic acid piperidinium salt in the presence of water, and distilling the aqueous layer to recover the by-produced piperidine.
CONSTITUTION: An alkali metal hydroxide is added to a solution of an N,N- pentamethylenethiolcarbamic acid piperidinium salt in an organic solvent (e.g. hydrophobic aromatic hydrocarbon, aliphatic hydrocarbon, ether, etc.) at a molar ratio of 1:(1W1.5), and reacted with each other to obtain the titledsubstance. The aqueous layer is distilled to recover the fraction containing by produced piperidine, and the aqueous layer containing the titled substance (the compound of formula) is obtained as the distillation residue. The distillation is carried out at the column bottom temperature of ≤70°C under reduced pressure. The concentration of the alkali metal salt in the aqueous layer containing the titled substance is 40W50wt%.
USE: Used as synthetic intermediate of herbicide.
COPYRIGHT: (C)1986,JPO&Japio
摘要翻译：目的：为了获得含有标题物质的含水层，在水存在下，通过碱金属氢氧化物与N，N-五亚甲基硫代氨基甲酸哌啶鎓盐的有机溶剂溶液反应，蒸馏除去副产物哌啶。构成：将碱金属氢氧化物以1：（1-1.5）的摩尔比加入到N，N-五亚甲基硫代氨基哌啶鎓盐的有机溶剂（例如疏水性芳族烃，脂族烃，醚等）的溶液中），并进行反应，得到标题物质。蒸馏水层以回收由产生的哌啶含有的级分，得到含有标题物质（式的化合物）的水层作为蒸馏残渣。蒸馏在塔底温度<70℃，减压下进行。含有标题物质的水层中的碱金属盐的浓度为40〜50重量％。用途：用作除草剂的合成中间体。

2. 发明专利

JPS5759826A Preparation of aromatic oily substance composed mainly of trimethylcyclododecadiene carbaldehyde 失效
标题翻译：芳香族油性物质的制备主要由三甲基氯化碳二苯醚
公开(公告)号：JPS5759826A
公开(公告)日：1982-04-10
申请号：JP13703380
申请日：1980-09-30
申请人： Mitsubishi Petrochem Co Ltd
发明人： TAKEDA MAKOTO , IWANE HIROSHI , OOKAGO YUUJI , KUJIRA KATSUFUMI
IPC分类号： C11D3/50 , A61K8/33 , A61Q13/00 , B01J23/00 , B01J23/46 , B01J27/00 , B01J27/06 , B01J27/20 , B01J31/00 , B01J31/04 , B01J31/16 , C07B61/00 , C07C45/00 , C07C45/50 , C07C47/33 , C07C47/43 , C07C67/00 , C11B9/00 , C11D9/44
CPC分类号： Y02P20/52
摘要： PURPOSE: To prepare the titled substance useful as an aromatic, etc., by reacting 1,6,9-trimethyl-1,5,9-cyclodedecartriene which is available in a large amount at a low cost, with CO and H
2 in the presence of a hydroformylation catalyst.
CONSTITUTION: An aromatic oily substance containing 2,6,9-trimethyl-5,9-cyclododecadiene carbaldehyde is prepared by reacting 1,6,9-trimethyl-1,5,9-cyclodedecatriene with carbon monoxide and hydrogen in the presence of a hydroformylation catalyst such as a rhodium compound or a cobalt compound pref. at 50W70°C and 59W400kg/cm
2 G at a CO/H
2 molar ratio of 0.5W2. The reaction pressure can be lowered by adding 1W10
3 mol, pref. 10W10
2 mol of a tert-phosphine to 1mol of the catalyst.
COPYRIGHT: (C)1982,JPO&Japio
摘要翻译：目的：为了制备作为芳香族等有用的标题物质，可以通过以低成本获得大量的1,6,9-三甲基-1,5,9-环己二烯与CO和H 2反应，存在加氢甲酰化催化剂。构成：含有2,6,9-三甲基-5,9-环十二碳二烯甲醛的芳族油性物质是通过使1,6,9-三甲基-1,5,9-环己基三烯与一氧化碳和氢在存在下加氢甲酰化催化剂如铑化合物或钴化合物。在50-70℃和59-400kg / cm 2 G，CO / H 2摩尔比为0.5-2。反应压力可以通过加入1-10 3mol， 10-10微摩尔的叔膦至1摩尔的催化剂。

3. 发明专利

JPS5976081A Preparation of thiopheneacetic acid or its derivative 失效
标题翻译：二苯甲酸或其衍生物的制备
公开(公告)号：JPS5976081A
公开(公告)日：1984-04-28
申请号：JP18525682
申请日：1982-10-21
申请人： Mitsubishi Petrochem Co Ltd
发明人： TAKEDA MAKOTO , IWANE HIROSHI , KUJIRA KATSUFUMI
IPC分类号： C07D333/24 , B01J31/00 , B01J31/22 , B01J31/24 , C07B61/00 , C07D333/32
CPC分类号： Y02P20/52
摘要： PURPOSE: To obtain the titled compound useful as an intermediate for drugs in high yield with preparing a small amount of by-products, by reacting thiophene methanol or its derivative with CO, water, an alcohol, etc. in the presence of a palladium catalyst.
CONSTITUTION: A thiophene methanol or its derivative shown by the formula I (R
1 is H, or alkyl; R
2 is H, halogen, etc.) is reacted with CO and water, an alcohol, or a phenol shown by the formula R
3 -OH(R
3 is H, etc.) in the presence of a palladium catalyst in the absence of a solvent or in a solvent such as hexane, etc. usually at 40W180°C, to give the desired compound shown by the formula II. In order to raise the reaction rate, an acidic compound such as a hydrogen halide, etc. as a cocatalyst is preferably added to the reaction system.
EFFECT: The desired compound is obtained by using relatively inexpensive safe raw materials for the reaction by one step and simple operation.
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：目的：通过在钯催化剂存在下，噻吩甲醇或其衍生物与CO，水，醇等反应，得到高产量的药物中间体，制备少量副产物，得到标题化合物。构成：式I表示的噻吩甲醇或其衍生物（R 1是H或烷基; R 2是H，卤素等）与CO和水，醇或苯酚显示反应在不存在溶剂的情况下，在钯催化剂存在下，或在溶剂如己烷等中，通式为R 3 -OH（R 3为H等），通常为40-180℃，得到式II所示的所需化合物。为了提高反应速度，优选在反应体系中添加作为助催化剂的卤化氢等酸性化合物。效果：通过使用相对便宜的用于反应的安全原料通过一步和简单的操作获得所需化合物。

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