![]() Method of obtaining chlorofluoroalkyl esters
专利摘要:
Flouro-halo-ethers of general formula: (R)nC(F)m-O-CAF-CAF2 wherein R is a partly or completely halogenated hydrocarbon, alkyl monoether or alkyl polyether radical, A is either chlorine or bromine, n is an integer selected between 1 and 2, m is an integer equal to 3-in. The value n = 2 comprises the compounds wherein C is a part of a cyclic ring. 公开号:SU1533624A3 申请号:SU864027584 申请日:1986-05-16 公开日:1989-12-30 发明作者:Гульелмо Джорджио;Гамбаретто Джампаоло 申请人:Аусимонт С.П.А. (Фирма); IPC主号:
专利说明:
The invention relates to a process for the preparation of new chlorofluoroalkyl ethers of the general formula R-0-CC1F-CC1F ,,, where R - CC1G2-СРг-, CF, -CF2 -CF2 CF3 -CFZ-, which can be used to make the corresponding vinyl ethers. The purpose of the invention is to develop a process for the preparation of new chlorofluoroalkyl ethers, the use of which makes it possible to obtain the corresponding vinyl ethers in a simpler way. PRI me R 1. In the upper part of a metal tubular reactor having an internal diameter of 1 cm and a length of 1300 cm, cooled to a temperature –OZ, a gas mixture Ng / C4F, OF is fed at an absolute pressure of 110 KPa at 20% by volume of CZF5OF ; at a distance of approximately 300 cm from the top, a gas mixture of C2ClFr / CC1F CC1F is fed at 20 ov.%. The speed of the two streams is adjusted at 18.7 Ml / h each. The stream leaving the reactor is cooled to -80 ° C and the condensate is distilled. After 6 hours of continuous feed, 72 g of fraction are obtained; 99% by weight of CrP5 OCC1F - CC1Pg. The output is 25 mol D. The product is identified by mass spectrometry and it has a bp. 60- 624. Elementary analysis of the product is as follows, wt%: C CljFjO; C 16.7; Cl 2.7; F 53.0; about 5.6. For the dehalogenation of this product, a flask with a capacity of 100 ml is used, which is equipped with a distillation column, a discharge tube and a condenser. 50 ml of dimethyl sulfoxide, 5 g of K2CO3, 1 g of K, 5 g of zinc powder and 20 g of product are loaded into the flask at room temperature with stirring. The mixture is heated to 55 ° C and after 4 hours 13.5 Cg F5 is collected with a yield of 89.7%. The product has bp. 9 ° C. Elementary analysis of the following, wt.%: C4F90; C 22.2; C1 70, bi O 7L EXAMPLE 2 A test is carried out as in the example, however, the gas mixture N2 / CClFe-CF2OF is loaded into the upper part of the reactor at 20% by volume of CC1F2-C1 g OF. After 10 hours of continuous feed and subsequent distillation, 31 are obtained. g product with a yield of 99%, which is identified by mass spectrophotometric analysis as CC1Rg-CPG-CC1R-CCi, and the product has a so-called bake. 90-92 ° C. Elementary analysis of the following, wt.%: C C1SF70; C 15.8; C1 35.1; F, 8; 0 5.3. The corresponding vinyl ester CC1F2-CK2-O-CF CF2 is obtained from this product by dehalogenation, as described in Example 1, with a yield of 88.5%. Vinyl ether has a so-called boiling point. k2-. Elementary analysis of the following, wt.%: C4C1FT0: C 20.6; C1 15.3; F 57.2; 0 6.9. PRI me R 3. The test was carried out as in Example 1, however 0 0 five five In the upper part of the reactor, the gas mixture Nj, / CF3-CFt-CF2-OF at 20 vol.% CF3 -CFZ CFZ -OF. After 10 hours of continuous feed and subsequent distillation, AO g of product is obtained at a yield of 99%, which is identified by mass spectrophotometric analysis as CF9-CFt-CFz-0-CClF-CClFa. The b.p. of product is 80-82 ° C. I Elemental analysis of the product is as follows, wt%: C5C12F, 00: C 17.8; C1 21.1; F 56,4; 0 ", 7. The corresponding vinyl ether CFj-CFz-CF2-0-CF CF2 is obtained from this product by dehalogenation as described in Example 1, and the yield of the ester is 91.8%. 0 It has a boiling point. C. Elemental analysis of the following, wt.%: C5F100. C 22.6; F 71; about b, oh Thus, the synthesized chlorofluoroalkyl ethers make it possible to obtain rather simply and with high yield the corresponding vinyl ethers, while the known method required the use of stoichiometric amounts of compounds of the formula Rf-, which were heated in the presence of a solid oxide of the element of groups 11-A, 111 -8, IV-A.
权利要求:
Claims (1) [1] Invention Formula The method of obtaining chlorofluoroalkyl ethers of the general formula R - O - CC1F - CC1F2, where R - CC1Гг-СРг-, CF3-CF -CFZ, CK3-CGG-, characterized in that the halogen compound of the general formula R - CFЈOF, where R is CF3, CClFj, CF} -CF2-, is reacted with a halo-olefin of the formula in the presence of an inert gas at a low temperature.
类似技术:
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同族专利:
公开号 | 公开日 AU5737186A|1986-11-20| IL78784D0|1986-08-31| IT8520781D0|1985-05-17| EP0201871A1|1986-11-20| AU584196B2|1989-05-18| IT1187674B|1987-12-23| AT36313T|1988-08-15| JPS625932A|1987-01-12| ZA863504B|1986-12-30| EP0201871B1|1988-08-10| DE3660490D1|1988-09-15| KR860008964A|1986-12-19|
引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题 US3558721A|1967-12-22|1971-01-26|Allied Chem|Method for the preparation of fluorinated ethers| US4334105A|1979-04-25|1982-06-08|Airco, Inc.|Method for the dehalogenation of ethers| GB2148286B|1983-10-24|1987-09-30|Occidental Chem Co|Preparation of chlorotrifluoroethylene telomers with fluoroxytrifluoromethane and bisfluoroxydifluoro methane|IT1213536B|1986-11-14|1989-12-20|Ausimont Spa|2-BROMO, 1 ', 2', - DICHLORO-PERFLUORO DIETYL-ETHER AND PROCEDURE FOR LASUA PREPARATION.| US5292961A|1986-11-14|1994-03-08|Ausimont S.P.A.|Process for the preparation of halogenated polyethers| US5457242A|1986-11-14|1995-10-10|Ausimont S.R.L.|2-bromo,1',2'-dichloroperfluoro diethyl ether and process for preparing same| IT1198285B|1986-11-14|1988-12-21|Ausimont Spa|PROCEDURE FOR THE PREPARATION OF ETHER FLUOROALOGEN FROM FLUOROXY-COMPOUNDS AND ALGENATE OLEFINS| IT1198284B|1986-11-14|1988-12-21|Ausimont Spa|PROCEDURE FOR THE PREPARATION OF HALOGEN POLYETERS| US5001980A|1988-12-29|1991-03-26|Komori Printing Machinery Co., Ltd.|Delivery apparatus for sheet-fed printing press| IT1246357B|1990-07-12|1994-11-17|Ausimont Spa|PROCESS FOR THE PREPARATION OF PERFLUOROALCOXYSULPHONIC COMPOUNDS| US6388139B1|1997-11-05|2002-05-14|E. I. Du Pont De Nemours And Company|Production of perfluoroethers| ITMI20020198A1|2002-02-05|2003-08-05|Ausimont Spa| haloethers| ITMI20021782A1|2002-08-06|2004-02-07|Ausimont S P A Ora Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI.| ITMI20030444A1|2003-03-11|2004-09-12|Solvay Solexis Spa|PROCESS TO PREPAREFLUOROALOGENOETERI.| ITMI20040132A1|2004-01-29|2004-04-29|Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI| ITMI20040133A1|2004-01-29|2004-04-29|Solvay Solexis Spa|PROCESS TO PREPARE FLUOROALOGENOETERI| US7247757B2|2004-10-06|2007-07-24|Fujifilm Corporation|Method of producing a fluorine-containing vinyl ether compound| ITMI20052455A1|2005-12-22|2007-06-23|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF FLUOROALOGENOETERI| ITMI20052456A1|2005-12-22|2007-06-23|Solvay Solexis Spa|PROCEDURE FOR THE PREPARATION OF FLUOROALOGENOETERI| RU2696871C2|2017-12-08|2019-08-07|Федеральное государственное бюджетное учреждение науки Институт элементоорганических соединений им. А.Н. Несмеянова Российской академии наук |2-bromotetrafluoroethylperfluoroalkyl esters for producing emulsions for medical and biological purposes|
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申请号 | 申请日 | 专利标题 IT20781/85A|IT1187674B|1985-05-17|1985-05-17|ETHI HALOGEN FLUOR AND PROCEDURE TO OBTAIN THEM| 相关专利
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