CN101462980B - Industrial production method of 2,6-difluorobenzamide - Google Patents
Industrial production method of 2,6-difluorobenzamide Download PDFInfo
- Publication number
- CN101462980B CN101462980B CN 200910028785 CN200910028785A CN101462980B CN 101462980 B CN101462980 B CN 101462980B CN 200910028785 CN200910028785 CN 200910028785 CN 200910028785 A CN200910028785 A CN 200910028785A CN 101462980 B CN101462980 B CN 101462980B
- Authority
- CN
- China
- Prior art keywords
- hydrolysis
- difluorobenzamide
- kettle
- difluorobenzonilyile
- hydrogen peroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses an industrial production method of 2, 6-difluorobenzamide and relates to the industrial synthesis method of chemical raw material. 2, 6-difluorobenzonitrile is used as raw material, and alkali is used as a catalyst for synthesizing the 2, 6-difluorobenzamide by hydrolysis. The invention is characterized in that the other raw material participating in the hydrolysis is hydrogen peroxide. In the method, the raw materials participating in the hydrolysis are the 2, 6-difluorobenzonitrile and the hydrogen peroxide, and the alkali is used as the catalyst, so that the product quality is stable, the yield is as high as 1.04, the purity is 99 percent, the production environment has no pollution, the reaction condition is mild, time is short, energy is saved, requirement for the equipment is not high and the production is easy.
Description
Technical field
The present invention relates to the industrial preparative method of industrial chemicals, particularly produce intermediate 2, the synthesis technology field of 6-difluorobenzamide as agricultural chemicals, medicine, liquid crystal material.
Background technology
2,6-difluorobenzamide finished product is white, needle-shaped crystals, is agricultural chemicals, medicine, liquid crystal material production intermediate.Mostly adopt now difluorobenzonilyile to be hydrolyzed, method for hydrolysis has two kinds, and a kind of is to adopt acid catalyzed process, and another kind is to adopt the base catalysis method.The method product of existing two kinds of hydrolysis all needs to neutralize, and expends a large amount of acid or alkali consumption, also produces a large amount of abraum salts, and simultaneously, environmental pollution is serious.
Summary of the invention
The present invention seeks to invent that a kind of material loss is few, energy-conservation, the production process environmental protection 2, the industrialized preparing process of 6-difluorobenzamide.
Be raw material with 2,6-difluorobenzonilyile, highly basic is catalyzer, hydrolysis 2, and the 6-difluorobenzamide is characterized in that another raw material that participates in being hydrolyzed is hydrogen peroxide.
Of the present invention 2, the mass ratio of 6-difluorobenzonilyile, highly basic and hydrogen peroxide is 100: 1～10: 200～300.
Concrete grammar is: first 2,6-difluorobenzonilyile is placed in the hydrolysis kettle, under the agitation condition highly basic is added hydrolysis kettle in batches, adopting steam to make the interior hydrolysis temperature of hydrolysis kettle is 20～50 ℃, drips hydrogen peroxide again, and the pH value with material in the alkali adjusting hydrolysis kettle in hydrolytic process is 8～10, in hydrolysis kettle 2, during 6-difluorobenzonilyile mass content＜0.5%, hydrolysis finishes, and continues to stir, and kept the hydrolysis temperature in the kettle 0.5～2 hour, then, be cooled to below 10 ℃, take out solid matter; Take water as washing composition, after adopting suction method to wash to go out water ph value and be 7～8 to whizzer, solid matter is placed drying in oven, namely get 2,6-difluorobenzamide.
The raw material that the present invention participates in being hydrolyzed is 2,6-difluorobenzonilyile and hydrogen peroxide, and highly basic is catalyzer, and constant product quality, yield are up to 95%, purity 99%, production environment is pollution-free, and reaction conditions is gentle, and the time is short, save energy, less demanding to equipment is easy to produce.
In addition, temperature is 70～100 ℃ in the baking oven of the present invention.
Described catalyzer is sodium hydroxide.
Embodiment
Production stage:
1, gets the raw materials ready
Take by weighing respectively 2,6-difluorobenzonilyile 100kg, sodium hydroxide 1～10kg, hydrogen peroxide 200～300kg.
2, hydrogen peroxide is extracted in the header tank, stand-by.
3, open hydrolysis kettle, add 2,6-difluorobenzonilyile, start and stir setting, add in batches sodium hydroxide.
4, adopt steam to make the hydrolysis temperature in the kettle be upgraded to 20～50 ℃, slowly drip hydrogen peroxide, in hydrolysis kettle 2, when 6-difluorobenzonilyile content was lower than 0.5%, reaction finished.In the reaction process, the pH value of regulating material in the hydrolysis kettle with sodium hydroxide is 8～10, and in hydrolysis kettle 2, during 6-difluorobenzonilyile mass content＜0.5%, hydrolysis finishes.Continue to stir, and kept the hydrolysis temperature in the kettle 0.5～2 hour.
5, being cooled to the hydrolysis temperature in the kettle is below 10 ℃ the time, takes out solid matter.
6, take water as washing composition, after adopting suction method repetitive scrubbing to whizzer to go out water ph value to be 7～8, solid matter is placed 70～100 ℃ drying in oven, namely get 2,6-difluorobenzamide.
The finished product 2,6-difluorobenzamide content 〉=99%.
Claims (2)
1.2, the industrialized preparing process of 6-difluorobenzamide, with 2, the 6-difluorobenzonilyile is raw material, sodium hydroxide is catalyzer, with synthetic 2, the 6-difluorobenzamide of hydrogen peroxide hydrolysis, it is characterized in that: first with 2, the 6-difluorobenzonilyile places in the hydrolysis kettle, under the agitation condition sodium hydroxide is added hydrolysis kettle in batches, and adopting steam to make the interior hydrolysis temperature of hydrolysis kettle is 20～50 ℃, drip again hydrogen peroxide, the pH value of regulating material in the hydrolysis kettle with alkali in hydrolytic process is 8～10, in hydrolysis kettle 2, during 6-difluorobenzonilyile mass content＜0.5%, hydrolysis finishes, continue to stir, and kept the hydrolysis temperature in the kettle 0.5～2 hour, then, be cooled to below 10 ℃, take out solid matter; Take water as washing composition, after adopting suction method to wash to be 7～8 to whizzer water outlet pH value, solid matter is placed drying in oven, namely get 2,6-difluorobenzamide; Described 2, the mass ratio of 6-difluorobenzonilyile, sodium hydroxide and hydrogen peroxide is 100: 1～10: 200～300.
2. described 2 according to claim 1, the industrialized preparing process of 6-difluorobenzamide is characterized in that temperature is 70～100 ℃ in the baking oven.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910028785 CN101462980B (en) | 2009-01-05 | 2009-01-05 | Industrial production method of 2,6-difluorobenzamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910028785 CN101462980B (en) | 2009-01-05 | 2009-01-05 | Industrial production method of 2,6-difluorobenzamide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101462980A CN101462980A (en) | 2009-06-24 |
| CN101462980B true CN101462980B (en) | 2013-01-09 |
Family
ID=40803801
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200910028785 Expired - Fee Related CN101462980B (en) | 2009-01-05 | 2009-01-05 | Industrial production method of 2,6-difluorobenzamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101462980B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4691669B2 (en) | 2007-08-22 | 2011-06-01 | アストラゼネカ・アクチエボラーグ | Cyclopropylamide derivative |
| TW201039825A (en) | 2009-02-20 | 2010-11-16 | Astrazeneca Ab | Cyclopropyl amide derivatives 983 |
| KR20130002316A (en) | 2010-02-18 | 2013-01-07 | 아스트라제네카 아베 | New crystalline form of a cyclopropyl benzamide derivative |
| CN103232359A (en) * | 2013-05-09 | 2013-08-07 | 温州大学 | Environmental-friendly nitrile hydrolysis method |
| CN108623491B (en) * | 2017-03-24 | 2020-12-22 | 联化科技股份有限公司 | Preparation method of halogenated benzamide compound |
| CN111116399A (en) * | 2019-12-20 | 2020-05-08 | 杨向党 | Process for producing 2, 6-difluorobenzamide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580042A (en) * | 2003-08-15 | 2005-02-16 | 中国科学院动物研究所 | Substituted benzoyl urea insect growth regulator synthesizing method |
-
2009
- 2009-01-05 CN CN 200910028785 patent/CN101462980B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580042A (en) * | 2003-08-15 | 2005-02-16 | 中国科学院动物研究所 | Substituted benzoyl urea insect growth regulator synthesizing method |
Non-Patent Citations (1)
| Title |
|---|
| 徐秀军.二氟代苯甲酰胺的合成.《河北化工》.1998,(第4期),第33-35页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101462980A (en) | 2009-06-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101462980B (en) | Industrial production method of 2,6-difluorobenzamide | |
| CN102321028B (en) | Method for synthesizing 2-methyl-5-nitroimidazole-1-ethanol | |
| CN102260174B (en) | Application of solid acid catalyst in preparation of 2,5-dichloronitrobenzene | |
| CN101659606A (en) | Method for producing calcium formate by using industrial waste liquid | |
| CN103382166B (en) | Method for preparing 2, 6-dichlorobenzonitrile | |
| CN103396306A (en) | Cardanol Gemini polyoxyethylene ether carboxylate and preparation method thereof | |
| CN1990460B (en) | Comprehensive treatment of glycine crystallization mother liquid | |
| CN113200862B (en) | Synthetic process of sodium p-nitrophenolate | |
| CN102557077B (en) | Method for producing ammonium sulfate by using calcium sulfate waste residues produced in lactic acid production | |
| CN106336341A (en) | Process for synthesizing ethyl chloride | |
| CN109400492B (en) | Preparation method of tetrasodium aspartate diacetate | |
| CN103102327A (en) | Preparation method of rubber accelerator DZ (N,N-Dicyclohexyl-2-benzothiazolsulfene amide) | |
| CN207793119U (en) | The device of continuous production high-quality N- fatty acyl amino-acid salt surfactants | |
| CN111825217A (en) | Acetic acid-magnesium acetate liquid carbon source and production process and application thereof | |
| CN106430247A (en) | Method for preparing high-concentration sodium hydroxide by ultrasonically intensifying sodium sulfate | |
| CN108203392A (en) | A kind of process for cleanly preparing of glycine in coproduction with ammonium chloride | |
| CN101786960B (en) | Method for preparing betaine hydrochloride | |
| CN101863793A (en) | Synthesizing method of N-methyl glucamine | |
| CN102329251A (en) | Method for chemically synthesizing p-guanidinobenzoic acid | |
| CN104447290A (en) | Method for preparing 2,4-dichlorophenoxyacetic acid | |
| CN109096048A (en) | A kind of method of hydration method synthesizing dihydromyrcenol | |
| CN102675232B (en) | Synthetic method of 4-(6-chlorine-quinoxaline-2-yloxy)-phenol | |
| CN101941916A (en) | Method for refining high-purity N, N-diethyl-3-methylbenzamide | |
| CN102030341A (en) | Preparation method of medium silicon X molecular sieve MSX (medium silicon X) raw powder | |
| CN101100439A (en) | Technique for preparing serinol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130109 Termination date: 20180105 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |