CN102060736A - Method for synthesizing propoxur - Google Patents
Method for synthesizing propoxur Download PDFInfo
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- CN102060736A CN102060736A CN2009102197738A CN200910219773A CN102060736A CN 102060736 A CN102060736 A CN 102060736A CN 2009102197738 A CN2009102197738 A CN 2009102197738A CN 200910219773 A CN200910219773 A CN 200910219773A CN 102060736 A CN102060736 A CN 102060736A
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- propoxur
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Abstract
The invention relates to a method for synthesizing a pesticide, in particular to a method for synthesizing propoxur. The invention provides the method for synthesizing the propoxur, which is simple and has low pollution and high yield. The method comprises the following steps of: adding o-isopropoxy phenol and catalyst in a ratio of 1:0.001-0.05 into a glass reactor; stirring and cooling, and slowly dripping methylisocyanate (MIC), wherein the ratio of the phenol to the MIC is 1:1-1:1.2; and after the dripping is completed, reacting for 0.5 to 3 hours at the temperature of between 60 and 110 DEG C.
Description
Technical field:
The present invention relates to a kind of synthetic method of sterilant, more particularly, relate to the synthetic method of Propoxur.
Background technology:
Propoxur is a kind of carbamate insecticides, and the various sanitary insect pests that are mainly used in the cash crop pest control and eliminate family and public place have characteristics such as insecticidal spectrum is wide, residual effect length, killing rate height.
Present stage, the synthetic method of Propoxur has three kinds:
1. carbonochloridic acid ester method, this method method flow are complicated;
2. methylamino formyl chloride method, this method environmental pollution is more serious;
3. methyl isocyanate method, though this method method flow is simple, the three wastes are few, reaction yield is generally below 90%.
Summary of the invention:
The present invention is exactly at the problems referred to above, and the synthetic method of the Propoxur that a kind of method is simple, pollution is little, yield is high is provided.
In order to realize above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and method steps of the present invention is: in glass reactor, add adjacent isopropoxy phenol and catalyzer, n (phenol): n (catalyzer)=1: 0.001～0.05; Stir cooling, slowly drip methyl isocyanate (MIC), n (phenol): n (MIC)=1: 1～1: 1.2; After dropwising, react 0.5～3h down at 60～110 ℃.
Reaction equation is:
Beneficial effect of the present invention:
1. the present invention is simple to operate, the reaction times is short, temperature of reaction is low;
2. yield of the present invention is 99.2%, is beneficial to suitability for industrialized production.
Embodiment:
Method steps of the present invention is: in glass reactor, add adjacent isopropoxy phenol and catalyzer, n (phenol): n (catalyzer)=1: 0.001～0.05; Stir cooling, slowly drip methyl isocyanate (MIC), n (phenol): n (MIC)=1: 1～1: 1.2; After dropwising, react 0.5～3h down at 60～110 ℃.
Reaction equation is:
As a kind of preferred version, the present invention adopts following technical scheme, n (phenol): n (catalyzer): n (MIC)=1: 0.005: 1.05; Temperature of reaction is 90～100 ℃, and the reaction times is 2h.
The present invention selects material molar ratio, catalyst levels, temperature of reaction, reaction times as the factor that influences reaction yield, can see Table 1, table 2, table 3, table 4.
The influence of table 1 feed molar comparison reaction yield
| Sequence number | N (phenol): n (MIC) | Content/% | Yield/% |
| 1 | 1∶1 | 96.8 | 98.8 |
| 2 | 1∶1.05 | 97.4 | 99.1 |
| 3 | 1∶1.1 | 97.3 | 99.2 |
| 4 | 1∶1.15 | 97.1 | 99.0 |
| 5 | 1∶1.2 | 97.2 | 99.1 |
Table 2 catalyst levels is to the influence of reaction yield
| Sequence number | N (phenol): n (catalyzer) | Content/% | Yield/% |
| 1 | 1∶0.05 | 96.8 | 99.4 |
| 2 | 1∶0.025 | 96.9 | 99.5 |
| 3 | 1∶0.01 | 97.1 | 99.3 |
| 4 | 1∶0.005 | 97.4 | 99.3 |
| 5 | 1∶0.0025 | 96.9 | 99.5 |
| 6 | 1∶0.001 | 95.4 | 99.8 |
Table 3 temperature of reaction is to the influence of reaction yield
| Sequence number | Temperature of reaction/℃ | Content/% | Yield/% |
| 1 | 60 | 85 | 96.5 |
| 2 | 80 | 90 | 92 |
| 3 | 90 | 97.4 | 99.3 |
| 4 | 100 | 97.2 | 99.4 |
| 5 | 110 | 96.5 | 98.5 |
Table 4 reaction times is to the influence of reaction yield
| Sequence number | Reaction times/h | Content/% | Yield/% |
| 1 | 0.5 | 96.4 | 98.5 |
| 2 | 1.5 | 97.1 | 99.1 |
| 3 | 2 | 97.5 | 99.4 |
| 4 | 2.5 | 97.2 | 99.1 |
| 5 | 3.0 | 97.1 | 99.05 |
Claims (3)
1. the synthetic method of a Propoxur is characterized in that, the present invention adopts following technical scheme, and method steps of the present invention is: in glass reactor, add adjacent isopropoxy phenol and catalyzer, n (phenol): n (catalyzer)=1: 0.001～0.05; Stir cooling, slowly drip methyl isocyanate (MIC), n (phenol): n (MIC)=1: 1～1: 1.2; After dropwising, react 0.5～3h down at 60～110 ℃.
Reaction equation is:
2. the synthetic method of a kind of Propoxur according to claim 1 is characterized in that, method steps of the present invention is: n (phenol): n (catalyzer): n (MIC)=1: 0.005: 1.05.
3. the synthetic method of a kind of Propoxur according to claim 1 is characterized in that, method steps of the present invention is: temperature of reaction is 90～100 ℃, and the reaction times is 2h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102197738A CN102060736A (en) | 2009-11-11 | 2009-11-11 | Method for synthesizing propoxur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102197738A CN102060736A (en) | 2009-11-11 | 2009-11-11 | Method for synthesizing propoxur |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102060736A true CN102060736A (en) | 2011-05-18 |
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ID=43996260
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102197738A Pending CN102060736A (en) | 2009-11-11 | 2009-11-11 | Method for synthesizing propoxur |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102060736A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674000A (en) * | 2017-09-07 | 2018-02-09 | 湖南化工研究院有限公司 | A kind of purification process of arprocarb |
| CN109384692A (en) * | 2018-12-12 | 2019-02-26 | 湖南海利常德农药化工有限公司 | A kind of preparation method of arprocarb |
-
2009
- 2009-11-11 CN CN2009102197738A patent/CN102060736A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107674000A (en) * | 2017-09-07 | 2018-02-09 | 湖南化工研究院有限公司 | A kind of purification process of arprocarb |
| CN107674000B (en) * | 2017-09-07 | 2020-08-14 | 湖南化工研究院有限公司 | Method for purifying propoxur |
| CN109384692A (en) * | 2018-12-12 | 2019-02-26 | 湖南海利常德农药化工有限公司 | A kind of preparation method of arprocarb |
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Addressee: Li Jiabo Document name: Notification of Publication of the Application for Invention |
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Addressee: Li Jiabo Document name: Notification of before Expiration of Request of Examination as to Substance |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20110518 |