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81. 发明专利

JPS60181039A FLUORINE-CONTAINING DIENE COMPOUND 失效
公开(公告)号：JPS60181039A
公开(公告)日：1985-09-14
申请号：JP3837784
申请日：1984-02-29
申请人： DAIKIN IND LTD
发明人： ISHIKAWA NOBUO , KITATSUME TOMOYA
IPC分类号： C07D307/42 , C07B31/00 , C07B37/12 , C07C27/00 , C07C33/40 , C07C67/00
摘要： NEW MATERIAL:A fluorine-containing diene compound shown by the formula I [R is aliphatic or aromatic group which may have substituent group; R is H, or -CH(OH)R (R is aliphatic or aromatic or heterocyclic group which may have substituent group); Rf is fluorine-containing aliphatic group]. EXAMPLE:A compound shown by the formula II. USE:An intermediate for synthesizing various fluorine-containing organic compound having Rf in a desired position, namely a building block. PREPARATION:For example, phenylacetylene is reacted with trifluoroacetaldedyde to give carbinol, which is reacted with methanesulfonyl chloride in pyridine to give mesylate. This compound is then reacted with a Grignard reagent to give a novel allenylsilane, which is finally reacted with an aldehyde shown by the formula R CHO in the presence of tetrabutylammonium fluoride, to give a fluorine- containing diene compound shown by the formula I .

82. 发明专利

JPS59164753A Preparation of alpha-fluoroalkyl-beta-alkoxy(or hydroxy)-ester 失效
标题翻译：阿尔法 - 氟代烷基 - 羟基（或羟基） - 酯的制备
公开(公告)号：JPS59164753A
公开(公告)日：1984-09-17
申请号：JP3878683
申请日：1983-03-09
申请人： Daikin Ind Ltd
发明人： ISHIKAWA NOBUO , NAKAI TAKESHI
IPC分类号： C07C69/67 , C07C67/00 , C07C69/73
摘要： NEW MATERIAL:The α-fluoroalkyl-β-alkoxy(or hydroxy)carboxylic acid ester of formula I (R
1 and R
2 are a group selected from H, alkyl, phenyl and alkoxy; R
3 is H or alkyl; R
4 is alkyl; Rf is fluoroalkyl).
USE: Useful as a synthetic intermediate, etc. of a physiologically active substance having fluoroalkyl group.
PREPARATION: The compound of formula I can be prepared in high yield, by reacting the fluoro-ester of formula RfCH
2 COOR
4 with the silylating agent of formula (R)
3 SiOTf (Tf is trifluoromethanesulfonyl), and reacting the resultant fluoroalkylsilylketene acetal of formula II (R is alkyl) with the acetal of formula III or the carbonyl compound of formula IV.
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：新物质：式I的α-氟代烷基-β-烷氧基（或羟基）羧酸酯（R 1和R 2）是选自H，烷基，苯基和烷氧基的基团; R 3是H 或烷基; R 4是烷基; R f是氟代烷基）。用途：可用作具有氟烷基的生理活性物质的合成中间体等。制备：式I化合物可以通过使式RfCH 2 COOR 4的氟代酯与式（R）3 SiOTf（Tf是三氟甲磺酰基）的甲硅烷基化剂反应，并使所得到的氟代烷基甲硅烷基乙烯酮缩醛与式 II（R是烷基）与式III的缩醛或式IV的羰基化合物反应。

83. 发明专利

JPS5948089A Preparation of fluorine-containing alcohol 失效
标题翻译：含氟的醇的制备
公开(公告)号：JPS5948089A
公开(公告)日：1984-03-19
申请号：JP15101082
申请日：1982-08-31
申请人： Daikin Ind Ltd
发明人： ISHIKAWA NOBUO , KITATSUME TOMOYA
IPC分类号： C12P7/06 , C12R1/865
CPC分类号： Y02E50/17
摘要： PURPOSE: To prepare a fluorine-containing alcohol, easily, in high yield, by treating a fluorine-containing carbonyl compound with microorganisms.
CONSTITUTION: A fluorine-containing carbonyl compound of formula I [R
f is fluorine-containing aliphatic group, fluorine-containing oxoaliphatic group, or fluorine-containing aromatic group; R is (substituted) aliphatic group] [e.g. CF
3 (CF
2 )
2 -COCH
3 , etc.] is treated with microorganisms (e.g. baker's yeast) to obtain the fluorine-containing alcohol of formula II (R
f and R are same as defined above) [e.g. CF
3 (CF
2 )
2 CH(OH)CH
3 , etc.], easily, in high yield. The fluorine-containing alcohol prepared by this process can be used as a solvent as well as a synthetic intermediate of water- and oil-repellent, pharmaceuticals, agricultural chemicals, etc., and is useful also as a raw material of monomer for the preparation of fluorine-containing polymer and raw material of various esters.
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：目的：通过用微生物处理含氟羰基化合物，容易地以高产率制备含氟醇。构成：式I的含氟羰基化合物[Rf是含氟脂族基团，含氟脂族基团或含氟芳族基团; R是（取代的）脂族基] CF3（CF2）2-COCH3等]用微生物（例如面包酵母）处理，得到式II的含氟醇（Rf和R与上述相同）[例如， CF 3（CF 2）2 CH（OH）CH 3等]，容易，高产率。通过该方法制备的含氟醇可以用作溶剂以及拒水拒油剂，药物，农药等的合成中间体，并且也可用作制备单体的原料的含氟聚合物和各种酯的原料。

84. 发明专利

JPS5946273A Preparation of fluorine-containing heterocyclic compound 失效
标题翻译：含氟的杂环化合物的制备
公开(公告)号：JPS5946273A
公开(公告)日：1984-03-15
申请号：JP15100182
申请日：1982-08-31
申请人： Daikin Ind Ltd
发明人： ISHIKAWA NOBUO , TAKAOKA AKIO
IPC分类号： C07D277/64 , C07D235/10 , C07D263/56
摘要： PURPOSE: To prepare the titled compound having physiological activity and useful as various pharmaceuticals, agricultural chemicals, etc., in high yield, only by reacting a bifunctional amine with a fluorine-containing alkylamine under mild condition.
CONSTITUTION: The bifunctional amine of formula I (R
1 and R
2 are H or hydrocarbon group which may together form a ring optionally having a substituent group; Y is imino, O or S) (e.g. the compound of formula II) is made to react efficiently with equivalent amount of a fluorine-containing alkylamine of formula III (R
3 and R
4 are hydrocarbon group) [e.g. (C
2 H
5 )
2 NCF
2 CHF
2 , etc.] at room temperature to obtain the fluorine-containing heterocyclic compound of formula IV (e.g. the compound of formula V).
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：目的：仅在温和条件下使双官能胺与含氟烷基胺反应，以高产率制备具有生理活性的标题化合物，可用作各种药物，农药等。构型：式Ⅰ的双官能胺（R 1和R 2）是H或烃基，它们可以一起形成任选具有取代基的环; Y是亚氨基，O或S）（例如式II化合物）与等量的式III的含氟烷基胺（R 3和R 4是烃基）有效反应[例如（C 2 H 5）2 NCF 2 CHF 2等]，得到式Ⅳ的含氟杂环化合物（例如式Ⅴ化合物）。

85. 发明专利

JPS5946235A Preparation of fluorine-containing allyl alcohol 失效
标题翻译：含氟甲醇的制备
公开(公告)号：JPS5946235A
公开(公告)日：1984-03-15
申请号：JP15100982
申请日：1982-08-31
申请人： Daikin Ind Ltd
发明人： ISHIKAWA NOBUO , KITATSUME TOMOYA
IPC分类号： C07C29/38 , C07C27/00 , C07C33/42 , C07C67/00
摘要： PURPOSE: To prepare a fluorine-containing allyl alcohol in high yield, with an easily controllable reaction process, by reacting a halogenated vinyl compound with a fluorine-containing carbonyl compound in the presence of an active metal under the action of ultrasonic radiation.
CONSTITUTION: The compound of formula I (R is H or aliphatic group, e.g. ≤10C alkyl; X' is halogen) is made to react with a compound of formula R
f COR' (R
f is fluorine-containing aliphatic group such as ≤10C fluorine-containing alkyl or alkenyl; R' is H or aliphatic group, e.g. ≤10C alkyl or alkenyl) in the presence of an active metal such as Mg, Mn, Cd and/or Cr (II) under the action of ultrasonic radiation, thereby fully activating the active metal with the action of the ultrasonic radiation, and effectively producing the objective compound of formula II with an easy operation. The site- and stereo-selective introduction of fluoroalkyl group to allyl alcohol is useful for imparting the product with stability, physiological activity, etc.
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：目的：通过在超声波辐射的作用下，在活性金属存在下，使卤代乙烯基化合物与含氟羰基化合物反应，以高产率制备含氟烯丙醇。构成：使式I化合物（R为H或脂族基团，例如<= 10C烷基; X'为卤素）与式RfCOR'化合物反应（Rf为含氟脂族基团，例如<= 10 含氟烷基或烯基; R'是H或脂族基团，例如<= 10个烷基或链烯基）在活性金属如Mg，Mn，Cd和/或Cr（II）的存在下，在超声辐射的作用下从而通过超声辐射的作用完全活化活性金属，并且容易操作有效地制备式II的目标化合物。氟烷基对烯丙醇的位置和立体选择性引入可用于赋予产品稳定性，生理活性等。

86. 发明专利

JPS5939854A Trapping of enolate ion of fluorine-containing group- substituted malonic ester 失效
标题翻译：含氟化合物 - 取代的马来酸酐的增强离子的捕获
公开(公告)号：JPS5939854A
公开(公告)日：1984-03-05
申请号：JP15100782
申请日：1982-08-31
申请人： Daikin Ind Ltd
发明人： ISHIKAWA NOBUO , NAKAI TAKESHI , INOUE YOSHIO
IPC分类号： C07C69/63 , B01J27/00 , B01J27/12 , B01J31/00 , B01J31/02 , C07C67/30
摘要： PURPOSE: To trap the titled ion useful as a raw material for polyester, etc. without eliminating an ion of fluoride, by reacting a fluorine-containing fatty group- substituted malonic ester with a weak base and/or the ion of fluoride.
CONSTITUTION: A fluorine-containing fatty group-substituted malonic ester shown by the formula I (Rf is fluorine-containing fatty group; R is fatty group, H or alkali metal) is treated with a relatively weak base (e.g., trialkylamine) and/or an ion of fluoride (e.g., F
- of CsF), so that a fluorine-containing enolate ion shwon by the formula II is trapped. Since H at the α-position of an ester (e.g., α-trifluoromethylmalonic ester) shown by the formula I is not completely pulled out by the use of the base, the ion of fluoride (F
- ) is not eliminated, the enolate ion can be trapped, it is reacted with various kinds of reactive substances, so the reaction is applied to organic syntheses.
COPYRIGHT: (C)1984,JPO&Japio
摘要翻译：目的：通过使含氟脂肪基取代的丙二酸酯与弱碱和/或氟离子反应，捕获可用作聚酯等的原料的标题离子，而不消除氟离子。构成：将式I所示的含氟脂肪族基取代的丙二酸酯（Rf为含氟脂肪族基团，R为脂肪族基，H或碱金属）用较弱的碱（例如三烷基胺）和/ 或氟离子（例如，CsF的F - ），使得被式II掺杂的含氟烯醇化物离子被捕获。由于式I所示的酯（例如，α-三氟甲基丙二酸酯）的α位上的H不能通过使用碱被完全拉出，因此不消除氟化物离子（F - ），烯醇化物离子可以被捕获，与各种反应物质反应，因此反应适用于有机合成。

87. 发明专利

JPS58152857A FLUOROACYLUREA COMPOUND OF FLUOROACYLTHIOUREA COMPOUND, AND THEIR CYCLIZED COMPOUND 失效
公开(公告)号：JPS58152857A
公开(公告)日：1983-09-10
申请号：JP3612582
申请日：1982-03-08
申请人： DAIKIN IND LTD
发明人： ISHIKAWA NOBUO , INOUE YOSHIO
IPC分类号： C07C275/50 , C07C67/00 , C07C325/00 , C07C335/26
摘要： NEW MATERIAL:The compound of formulaI(Rf and Rf are fluoroalkyl; R and R are alkyl; X is O or S) and its cyclized compound. EXAMPLE:The compound of formula II. USE:Useful as a synthetic intermediate of urea-based fluoro-compound. PROCESS:The compound of formulaIcan be prepared by the dehydrofluorination reaction of the fluoroalkylcarboxylic acid fluoride of formula III (Rf and Rf are preferably

88. 发明专利

JPS5892627A PREPARATION OF FLUORINE-CONTAINING ALIPHATIC UNSATURATED COMPOUND OR FLUORINE-CONTAINING AROMATIC COMPOUND 失效
公开(公告)号：JPS5892627A
公开(公告)日：1983-06-02
申请号：JP18945881
申请日：1981-11-26
申请人： DAIKIN IND LTD
发明人： ISHIKAWA NOBUO , KITATSUME TOMOYA
IPC分类号： C07C17/269 , B01J19/10 , B01J23/06 , B01J27/00 , B01J27/10 , B01J31/00 , B01J31/04 , B01J31/16 , C07B61/00 , C07C17/00 , C07C17/26 , C07C21/02 , C07C21/18 , C07C22/08 , C07C67/00
摘要： PURPOSE:To prepare the titled substance useful as a synthetic intermediate of pharmaceuticals and agricultural chemicals, etc., by reacting an F-containing aliphatic iodide with a halogen-substituted aliphatic unsaturated compound or a halogen-substituted aromatic compound in the presence of zinc powder and a pd catalyst under the irradiation with ultrasonic wave. CONSTITUTION:A compound of formula RfI (Rf is F-containing aliphatic group having C-number of preferably

89. 发明专利

JPS5857357A FLUORINE-CONTAINING AMIDINE AND ITS PREPARATION 失效
公开(公告)号：JPS5857357A
公开(公告)日：1983-04-05
申请号：JP15544181
申请日：1981-09-30
申请人： DAIKIN IND LTD
发明人： ISHIKAWA NOBUO , TAKAOKA AKIO
IPC分类号： C07D239/42 , A01N37/52 , A01N43/00 , C07C67/00 , C07C239/00 , C07C257/14 , C07D213/75 , C07D277/20 , C07D277/42 , C07D295/12
摘要： NEW MATERIAL:A compound of formulaI(Rf is fluoroalkyl including those having another substituent group introduced into a part thereof; R and R' are alkyl or together with N form a heterocyclic ring; R'' is alkyl or aryl or group forming a heterocyclic ring including those having a substituent group introduced into a part thereof). EXAMPLE:N-Phenyl-N',N'-diethyl-alpha,beta,beta,beta-tetrafluoropropionic acid amidine. USE:Useful as various medicines and agricultural chemicals. PROCESS:An unsaturated fluoroalkyl compound is reacted with a secondary amine of formula II, e.g. (CH3)2NH or (C2H5)2NH, and then with a parimary amine of the formula R''-NH2, e.g. CH3NH2 or C2H5NH2, to give the aimed compound of formulaI.

90. 发明专利

JPS57150631A PREPARATION OF ALPHA,BETA-CIS-DIFLUORO-BETA-ALKYL(OR ARYL)ACRYLIC ACID 失效
公开(公告)号：JPS57150631A
公开(公告)日：1982-09-17
申请号：JP3809281
申请日：1981-03-14
申请人： DAIKIN IND LTD
发明人： ISHIKAWA NOBUO , KITATSUME TOMOYA
IPC分类号： C07C57/52 , C07C51/00 , C07C57/60 , C07C67/00
摘要： PURPOSE:To prepare the cis-isomer of the titled compound, selectively, in high yield, by reacting 2-(alpha,beta,beta,beta-tetrafluoroethyl)benzoxazole with a metallic reagent, and hydrolyzing the product in the presence of an acid. CONSTITUTION:2-(alpha,beta,beta.beta-Tetrafluoroethyl)benzoxazole of formulaIis used as the starting raw material, and is made to react with a metallic reagent of formula RMgX[R is alkyl or (substituted-)aryl; X is halogen]or formula LiR. The resultant 2-[alpha,beta-cis-difluoro-beta-alkyl(or aryl)vinyl]benzoxazole of formula II is hydrolyzed in the presence of an acid (e.g. sulfuric acid, phosphoric acid, etc.) to obtain the objective alpha,beta-cis-difluoro-beta-alkyl(or aryl)acrylic acid. USE:Intermediate of organic fluorine compounds or monomer of fluorine-containing polymers.

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