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1. 发明专利

JPH02169544A PRODUCTION OF FLUORINE-CONTAINING ALKYL (METH)ACRYLATE 失效
公开(公告)号：JPH02169544A
公开(公告)日：1990-06-29
申请号：JP32193488
申请日：1988-12-22
申请人： TOSOH CORP
发明人： NAGASAKI YOSHITAKA , TAKAHASHI MITSURU
IPC分类号： C07C67/08 , C07B61/00 , C07C69/653
摘要： PURPOSE:To suppress side reaction and obtain the subject compound in high yield from a fluorine-containing alcohol and (meth)acrylic acid by reacting the above-menthioned alcohol with the methacrylic acid which is being added to a reaction system consisting of the afore-mentioned alcohol, azeotropic dehydrating solvent and acid catalyst. CONSTITUTION:(A) a compound expressed by formula I (n is a natural number of 1-4; Rf is 1-20C saturated or unsaturated fluorine-containing aliphatic group having straight or branched chain) and (B) acrylic or methacrylic acid are subjected to dehydrating condensation in the presence of (C) an acid catalyst to produce a compound, expressed by formula II (X is H or CH3) and useful as a special surfactant, etc. In the process, the raw material (B) is added to a reaction system consisting of the raw material (A), an azeotropic dehydrating solvent and the catalyst (C) at a constant rate of preferably 1.0-30mmol/min based on 1mol raw material (A) to quantitatively provide the objective compound with advantages, such as hardly any formation of by-products, simplified purification steps and facilitated isolating operation.

2. 发明专利

JPH02169553A PRODUCTION OF FLUORINE-CONTAINING CARBOXYLIC ACID AMMONIUM SALT 失效
公开(公告)号：JPH02169553A
公开(公告)日：1990-06-29
申请号：JP32193388
申请日：1988-12-22
申请人： TOSOH CORP
发明人： NAGASAKI YOSHITAKA , ODA YASUHIRO , TAKAHASHI MITSURU
IPC分类号： C07C211/62
摘要： PURPOSE:To produce the subject compound in high efficiency by reacting a fluorine-containing aliphatic halide with carbon dioxide in an organic solvent in the presence of zinc, hydrolyzing the reaction product, extracting with an organic solvent and introducing ammonia into the extracted liquid. CONSTITUTION:The objective compound is produced by (1) reacting a compound of formula PfX (Rf is 1-20C saturated or unsaturated fluorine-containing aliphatic group having straight or branched chain; X is Cl, Br or I) with carbon dioxide in an organic solvent (preferably an aprotic polar solvent, especially DMF) in the presence of zinc at 0-100 deg.C, (2) hydrolyzing the reaction mixture with a mineral acid optionally after removing the metal powder, (3) extracting with an organic solvent (preferably ether solvent), (4) washing the extracted liquid with an aqueous solution preferably containing a reducing agent and (5) introducing ammonia to the liquid to effect the reaction.

3. 发明专利

JPH02169528A PREPARATION OF FLUORINE-CONTAINING ALCOHOL 失效
公开(公告)号：JPH02169528A
公开(公告)日：1990-06-29
申请号：JP32193588
申请日：1988-12-22
申请人： TOSOH CORP
发明人： TAKAHASHI MITSURU , NAGASAKI YOSHITAKA , FUJII SATOSHI
IPC分类号： C07C29/147 , C07C31/38 , C07C31/40
摘要： PURPOSE:To provide the subject compound by reacting a fluorine-containing carboxylic acid ester with a metal boron hydride in a specific alcohol solvent and/or an ether solvent and subsequently in the solvent containing metal or ethanol. CONSTITUTION:When a compound of formula I (n is 1 or 2; R is fluorine- containing group having a 1-20C straight chain or branched chain) is reacted with a metal boron hydride (preferably sodium boron hydride), the compound of formula I is added to a solvent consisting of an alcohol of formula R OH (R is aliphatic group having a 3-5C straight chain or branched chain) and/or ether for the reaction an subsequently methanol or ethanol is added to the solvent is an amount of 1-30wt.% of the solvent to finish the reaction. The temperature of the reaction is preferably 20-80 deg.C. The method prevents a sudden exothermic reaction or the generation of dangerous hydrogen to provide the objective compound safely, simply and in a high yield.

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