专利摘要:
The method of producing 3,5-dichloroaniline by dechlorinating tetrachloroanilines in the liquid-acid phase in the presence of palladium as a catalyst under increased pressure and with heating means that, in order to increase the yield of the target product, the process is carried out in the presence of silver cocatalyst, In addition, a quantity of 0.20, 7 mol per 1 mol of palladium, at 160190 ° C and a pressure of 13-20 bar.
公开号:SU1199199A3
申请号:SU813316600
申请日:1981-08-01
公开日:1985-12-15
发明作者:Кордье Жорж;Фуийу Пьер
申请人:Рон-Пуленк Агрошими (Фирма);
IPC主号:
专利说明:

with

WITH QD
eleven
The invention relates to an improved process for the preparation of 3,5-dichloroaniline, which is an intermediate in the preparation of phytosanitary active substances,
The aim of the invention is to increase the yield of the target product.
The invention is illustrated by the following examples.
Example 1 A 250 cm autoclave with an inner coating of tantalum was charged with 0.42 g of 2,3,4,5-tetrachloroaniline, 0.07 g of a catalyst consisting of palladium and silver deposited on carbon activation (the specific surface area of the activated carbon was 1x100 weight content of palladium 3%, silver 2% j, 120 cm of an aqueous solution of hydrochloric acid with a concentration of 4 mol / l.
Autoclave zakryshayut, rinsed first with argon, then with hydrogen. Then, heating up to 160 ° C with spontaneous pressure increase, then, when this temperature is reached, hydrogen is introduced to a total pressure of (relative) 13 bar, of which 6 bar is the hydrogen partial pressure.
Substances are left to react under these conditions for 2 hours.
91992
Cool the liquid reaction mass, alkalinize with a solution of caustic soda (NaOH); the catalyst is separated by filtration 3,5-dichloraniline
extracted from the aqueous phase with methylene chloride; the solution in methylene chloride thus obtained is dried with sodium sulfate n-ad, the solvent is distilled off in vacuo.
The degree of conversion of tetrachloroaniline is 100%. The yield of the obtained 3,5-dichloraniline is 98%. The silver content of the medium is 0.00006 g-ion / l, Example 2, The process is carried out,
5 as described in example 1, with the replacement of the catalyst by another catalyst consisting of palladium (weight content 4%) and silver (weight content I%), carrier as in example 1, reaction time 1 h 10 min,
Under these conditions, 3,5-dichloroaniline is obtained with a yield of 87%, as a by-product, 3-chloroaniline G in a yield of 10%, the degree of conversion of tetrachloroanilium is 100%,
Example 3. In Example 1, replace 2,3,4,5-tetrachloroaniline with 2,3,5,6-tetrachloroyl, the process is carried out for 4 hours at 190 ° C under a total pressure of 20 bar, which is 10 bar by hydrogen. The yield of 3,5-dichloroaniline is 93%.
权利要求:
Claims (1)
[1]
(54) (57) METHOD FOR PRODUCING 3,5-Dichloroaniline by dechlorinating tetrachloroanilines in the liquid phase in the presence of palladium as a catalyst at elevated pressures and upon heating, characterized in that, in order to increase the yield of the target product, the process is carried out in the presence of cocatalyst silver, taken in an amount of 0.20.7 mol per 1 mol of palladium, at 16 ΟΙ 90 ° C and a pressure of 13-20 bar.
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同族专利:
公开号 | 公开日
FR2487824B1|1984-08-24|
DK343081A|1982-02-02|
KR830006171A|1983-09-17|
AT8249T|1984-07-15|
EP0045710A1|1982-02-10|
DE3164565D1|1984-08-09|
US4532350A|1985-07-30|
IL63298D0|1981-10-30|
HU187349B|1985-12-28|
DD201584A5|1983-07-27|
IE51458B1|1986-12-24|
BR8104982A|1982-04-20|
EP0045710B1|1984-07-04|
ES504474A0|1983-01-01|
CA1211127A|1986-09-09|
KR850000149B1|1985-02-28|
ES8306706A1|1983-01-01|
FR2487824A1|1982-02-05|
JPS5767542A|1982-04-24|
IE811739L|1982-02-01|
IL63298A|1984-12-31|
引用文献:
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BE792080A|1971-11-30|1973-05-29|Rhone Progil|DEHALOGENATION OF POLYHALOGENOUS AROMATIC COMPOUNDS|
DE2503187C3|1975-01-27|1979-05-31|Bayer Ag, 5090 Leverkusen|Process for the preparation of chlorine-meta-substituted anilines|
FR2403990B1|1977-09-22|1983-01-21|Rhone Poulenc Agrochimie|
FR2403991B1|1977-09-22|1981-01-30|Rhone Poulenc Agrochimie|
FR2449076B2|1979-02-15|1983-05-20|Rhone Poulenc Agrochimie|US4692554A|1983-10-18|1987-09-08|Mitsui Toatsu Chemicals, Inc.|Process for producing 1,3-bisbenzene|
US5051030A|1990-06-05|1991-09-24|Roy F. Weston, Inc.|Chemical detoxification process for treatment of soils contaminated with halogenated organic compounds|
US5089653A|1991-04-04|1992-02-18|Dow Elanco|Process for the selective reduction of the 4-halogen in 2,4-dihaloanilines|
CN109939713A|2019-03-20|2019-06-28|江苏扬农化工集团有限公司|A kind of preparation method of the loaded catalyst for chloronitrobenzene catalytic hydrogenation synthesis chloro aminobenzen|
法律状态:
优先权:
申请号 | 申请日 | 专利标题
FR8017325A|FR2487824B1|1980-08-01|1980-08-01|
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