CN1049652C - 2-methyl-2-methythio propionaldoxime prodn. process - Google Patents
2-methyl-2-methythio propionaldoxime prodn. process Download PDFInfo
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- CN1049652C CN1049652C CN97105869A CN97105869A CN1049652C CN 1049652 C CN1049652 C CN 1049652C CN 97105869 A CN97105869 A CN 97105869A CN 97105869 A CN97105869 A CN 97105869A CN 1049652 C CN1049652 C CN 1049652C
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- solvent
- methyl
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- propionaldoxime
- methylthio
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Abstract
The present invention relates to a preparation technological method of 2-methyl-2-methylthio propionaldoxime. A solvents I, isobutylene, sodium nitrite and industrial hydrochloric acid are put in a container, and 2-chloro-2-methyl-1-nitrosopropane dimers are prepared after the reaction; then, a solution of sodium methyl sulfate is put into the other container and is stirred, a suspension mixed by the 2-chloro-2-methyl-1-nitrosopropane dimers and a solvent II is put. After reactions end, a solvent III is added to the materials to carry out extraction treatment to prepare the 2-methyl-2-methylthio propionaldoxime. The preparation technological method is simple, and the prepared products are cheap.
Description
The present invention relates to 2-methyl-2-methylthio propionaldoxime method of manufacturing technology technical field.
Make the processing method of 2-methyl-2-methylthio propionaldoxime at present with iso-butylene, at home and abroad also do not have, only too harsh by the literature processing condition, make the product manufacture complexity, finished product price height.
The objective of the invention is to invent and a kind ofly make 2-methyl-2-methylthio propionaldoxime with iso-butylene, its method of manufacturing technology is simple, and the finished product price is low.
The present invention is achieved in that and loads onto agitator, thermometer, dropping funnel and gas introduction tube on tankage, normal pressure adds solvent I wherein earlier down, make in the container temperature drop low with the cooling of dry ice-ethanol bath, import iso-butylene, drop into solid sodium nitrite, start the reaction of agitation and dropping technical hydrochloric acid, remove cryostat then, heat up, unreacted excessive iso-butylene is reclaimed, remake vacuum filtration, filter cake washes with water, drying makes 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer, the treated solvent I that makes of vacuum filtration gained liquid; Sodium methyl mercaptide aqueous solution input is equipped with reflux condensing tube, in the tankage of thermometer and agitator, start stirring, thereby temperature of charge is risen with the water-bath heat temperature raising, the suspension input that 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer and solvent II are mixed wherein then, reaction finishes, in material, add solvent II I and carry out extraction treatment, by static or centrifugally operated layering, solvent II is recycled by simple distillation after the layering, extract layer is made solvent II I by vacuum distilling and is recycled, and the gained solids is 2-methyl-2-methylthio propionaldoxime simultaneously.
Described solvent I is C
1-C
4Alcohol, C
1-C
4A halogen or many haloalkanes.
Described solvent II is a water, C
1-C
4Alcohol or its mixed solution.
Described solvent II I is aromatic hydrocarbon or halogenated alkane.
Advantage of the present invention is: method of manufacturing technology is simple, and the finished product price is low.
Below in conjunction with embodiment, the present invention will be further described:
On 20 liters four-hole bottle, load onto agitator, thermometer, dropping funnel and gas introduction tube, normal pressure adds 2250 milliliters of industrial alcohols wherein earlier down, with dry ice-ethanol bath cooling, temperature drop is to below-13 ℃ in making, import 2000 gram iso-butylenes, 1452 gram solid sodium nitrites are once dropped into, start stirring, drip 4200 milliliters of 31% technical hydrochloric acids, react and remove cryostat after 1 hour, heat up, unreacted excessive iso-butylene is reclaimed, remake vacuum filtration, filter cake washs with 4000 ml waters, and drying makes 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer 6190 grams, the treated solvent I that makes of vacuum filtration gained liquid; 9545 milliliters of inputs of the sodium methyl mercaptide aqueous solution are equipped with reflux condensing tube, in another tankage of thermometer and agitator, start stirring, thereby temperature of charge is risen with the water-bath heat temperature raising, 8000 milliliters of inputs of suspension that 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer and solvent II are mixed wherein then, reaction finishes, in material, add solvent II I and carry out extraction treatment, by static or centrifugally operated layering, solvent II is recycled by simple distillation after the layering, extract layer is made solvent II I by vacuum distilling and is recycled, the gained solids is 2-methyl-2-methylthio propionaldoxime 2010 grams simultaneously, content 85.1%.
Its molecular formula is:
Claims (1)
1,2-methyl-2 methylthio propionaldoxime method of manufacturing technology is characterized in that: in the reactor that whipping appts, thermometer, dropping funnel and gas introduction tube are housed, add solvent I earlier, solvent I is selected from C
1-C
4Alcohol, C
1-C
4A halogen or many haloalkanes, with the cooling of dry ice-ethanol bath the temperature of reactor is reduced, import iso-butylene, drop into solid sodium nitrite, start stirring, drip the technical hydrochloric acid reaction; Remove cryostat then, heat up, unreacted excessive iso-butylene is reclaimed; Remake vacuum filtration, filter cake washes with water, and drying makes 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer; The treated recovery solvent of vacuum filtration gained liquid I; Sodium methyl mercaptide aqueous solution input is equipped with in the reactor of reflux condensing tube, thermometer and whipping appts, start stirring, thereby with heating in water bath material is heated up, then 2-chloro-2-methyl isophthalic acid-nitroso-group propane dipolymer and solvent II are mixed, solvent II is selected from water, C
1-C
4Alcohol or its mixed solution, will mix gained suspension and drop in this reactor and react; Reaction finishes, and adds solvent II I and carry out extraction treatment in this reactor, and solvent II I is selected from aromatic hydrocarbon or halogenated alkane, by static or centrifugally operated layering; After the layering solvent II is reclaimed by simple distillation, extract layer reclaims solvent II I by vacuum distilling, and distillation gained solids is 2-methyl-2-methylthio propionaldoxime.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97105869A CN1049652C (en) | 1997-05-29 | 1997-05-29 | 2-methyl-2-methythio propionaldoxime prodn. process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97105869A CN1049652C (en) | 1997-05-29 | 1997-05-29 | 2-methyl-2-methythio propionaldoxime prodn. process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1165816A CN1165816A (en) | 1997-11-26 |
| CN1049652C true CN1049652C (en) | 2000-02-23 |
Family
ID=5168163
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97105869A Expired - Fee Related CN1049652C (en) | 1997-05-29 | 1997-05-29 | 2-methyl-2-methythio propionaldoxime prodn. process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1049652C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4007277B2 (en) * | 2003-07-22 | 2007-11-14 | ブラザー工業株式会社 | Image forming apparatus |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3931331A (en) * | 1973-01-30 | 1976-01-06 | Allied Chemical Corporation | Process of preparing α-formyl sulfides and 2-hydrocarbylthioaldoximes therefrom |
-
1997
- 1997-05-29 CN CN97105869A patent/CN1049652C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3931331A (en) * | 1973-01-30 | 1976-01-06 | Allied Chemical Corporation | Process of preparing α-formyl sulfides and 2-hydrocarbylthioaldoximes therefrom |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1165816A (en) | 1997-11-26 |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |