专利摘要:
Preparation of 3-chloro-2-fluoro-5-(trifluoromethyl)pyridine in a liquid phase halogen exchange reaction from 2,3-dichloro-5-(trichloromethyl)pyridine in the absence of a catalyst.
公开号:SU1473711A3
申请号:SU853919403
申请日:1985-06-07
公开日:1989-04-15
发明作者:Е.Гатлин Джэнис;А.Ван Дорт Марк;Л.Фолькман Куртис
申请人:Дзе Дау Кемикал Компани (Фирма);
IPC主号:
专利说明:

one
The invention relates to organic synthesis, in particular to a method for producing 2, 3-dichloro-5- (trifluoromethyl) pyridine, which is a valuable intermediate product for the synthesis of herbicides.
The purpose of the invention is to simplify the process of obtaining 2, 3-dichloro-5- (trifluoromethyl) pyridine by carrying out the process in the liquid phase.
Example. 1209.5 g (4.52 mol) of 99% 2, 3-dichloro-5-trichloromethyl-pyridine is placed in a 1-liter Hasteloy-C reactor (Parr autoclave) equipped with a baking dish and connected
with refrigerators, heaters, means for regulating pressure and supplying hydrogen fluoride. The reactor is sealed, start heating and mixing. The pressure in the reactor is maintained within 1411.33 - -1549.22 kPa with nitrogen. When the temperature reaches 193 ° C, 46 g of hydrogen fluoride are added, after which the supply of HF is continued at an average consumption of 20 g / h (1.00 mol / h / 4.52 mol of pyridine), maintaining the temperature in the reactor at 186 ° C, pressure 1798 kPa and temperature in refrigerators 12 - 17 C. GLC analysis of the product
Ј
WITH
-sj
cm
3 14737114
after 38 hours, it showed a content of 5 mol.% Fed ,, pressure 83, 8 mass% 3-chloro-2-fluoro-5- (trifluorine 100-135.8 kPa, temperature 138-.
methyl) pyridine, tK4n 139-140 ° C, and 170 ° C, and anhydrous is continuously fed
8.0 wt.% 2,3-dichloro-5- (trifluorome-HCl for 23 h to obtain
thyl) pyridine, tkv, n 50-51 ° C at 5 2,3-dichloro-5- (trifluoromethyl) pyridine
6 mm Hg (90% yield).
In the second stage, the reactor is outdated. The overall yield is 85% for 61 hours, is teased and purged with nitrogen, after
权利要求:
Claims (1)
[1]
1. METHOD FOR PRODUCING 2,3-Dichloro-5- (triftho-methyl) pyridine based on a derivative of 5- (trifluoromethylpyridine) using a chlorinating agent when heated in the presence of
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同族专利:
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引用文献:
公开号 | 申请日 | 公开日 | 申请人 | 专利标题

GB1039987A|1964-03-17|1966-08-24|Pennwalt Corp|Fluoropyridines|
GB1272475A|1969-05-30|1972-04-26|Ici Ltd|Manufacture of fluoropyridines|
DE2862492D1|1977-08-12|1988-09-01|Ici Plc|Herbicidal halogenomethyl--pyridyloxy-phenoxy-alkanecarboxylic acids and derivatives, and processes of controlling unwanted plants therewith|
JPS5461183A|1977-10-21|1979-05-17|Ishihara Sangyo Kaisha Ltd|2-substituted-5-trifluoromethyl pyridine compounds|
JPS5585564A|1978-12-22|1980-06-27|Ishihara Sangyo Kaisha Ltd|Preparation of beta-trifluoromethylpyridine|
JPS55158979A|1979-05-29|1980-12-10|Seiko Epson Corp|Ink jet recording head|
EP0074192B1|1981-09-03|1986-12-30|Imperial Chemical Industries Plc|Chloro-trifluoromethyl pyridines|
US4567273A|1982-04-16|1986-01-28|The Dow Chemical Company|Liquid phase halogen exchange of pyridines to pyridines|
US4493932A|1982-09-13|1985-01-15|The Dow Chemical Company|Chlorine exchange for fluorine in 2-fluoro-pyridine compounds|
IL70307A|1982-11-26|1987-02-27|Dow Chemical Co|Preparation ofpyridines|EP0063872B1|1981-04-27|1985-07-17|Imperial Chemical Industries Plc|Process for the preparation of fluoromethyl pyridines and certain novel products obtained therefrom|
US4782161A|1987-10-21|1988-11-01|The Dow Chemical Company|Preparation of fluoropyridines|
US4999432A|1989-08-28|1991-03-12|Dowelanco|Fluorination with hydrogen fluoride|
CN107954924A|2016-10-18|2018-04-24|内蒙古佳瑞米精细化工有限公司|A kind of preparation method of the fluoro- 3- chloro-5-trifluoromethylpyridines of 2-|
CN107935920A|2017-11-30|2018-04-20|山东汇盟生物科技有限公司|The preparation method of 2 fluorine, 3 chlorine, 5 trifluoromethyl pyridine|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
US06/618,806|US4547577A|1984-06-08|1984-06-08|Preparation of pyridines|
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