CN106518910A - Method for preparing dialkyl chlorophosphate reagent through trimethylpyridine-phosphamide - Google Patents
Method for preparing dialkyl chlorophosphate reagent through trimethylpyridine-phosphamide Download PDFInfo
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- CN106518910A CN106518910A CN201510587629.5A CN201510587629A CN106518910A CN 106518910 A CN106518910 A CN 106518910A CN 201510587629 A CN201510587629 A CN 201510587629A CN 106518910 A CN106518910 A CN 106518910A
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- trimethylpyridine
- phosphamide
- chlorine
- reaction
- composition proportion
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Abstract
The invention discloses a method for preparing dialkyl chlorophosphate reagent through trimethylpyridine-phosphamide. The method comprises the following steps that the trimethylpyridine-phosphamide with a preset quantity is added into a reaction bulb; air in the reaction bulb is replaced with inert gas, cooling is conducted until the preset temperature is achieved; phosphoryl diamide is added into the reaction bulb drop by drop; when the reaction is finished, anhydrous solvent with a preset quantity is used for dilution, and products are filtered; and the products are subjected to concentration treatment, and dialkyl chlorophosphate is obtained. According to the method for preparing the dialkyl chlorophosphate reagent through the trimethylpyridine-phosphamide, any solvents are not used in the preparation process of the dialkyl chlorophosphate, the reaction can be completely conducted, the reaction time is short, and liquid waste is not generated. Generally, the purity of the products is sufficiently high, the requirement of general organic synthesis is met, and further distillation can be conducted if purity is not satisfactory.
Description
Technical field
A kind of a kind of the present invention relates to preparation method, more particularly to trimethylpyridine-phosphamide chlorine di(2-ethylhexyl)phosphate hydrocarbon
The method of base ester reagent.
Background technology
Chlorine dihydrocarbon is the important examination for synthesizing organic phosphorus compound, particularly phosphoric acid mixing ester compounds
Agent.Chlorine dihydrocarbon is prepared with gas chlorine source such as chlorine, phosgene reaction method by phosphite ester,
Need to remove the gas and acid dissolved in product with dry air and ceruse after reaction.Produce pollution environment
Solid waste.In prior art, using nitrogen-chloro-succimide or TCCA (Trichloroisocyanuric acid) as chlorine
Source.
During the present invention is realized, inventor has found that prior art at least has problems with：
The preparation method of prior art makees solvent using acetonitrile or toluene, produces unnecessary liquid debris；
Course of reaction needs heating, and the response time is long；The preparation method be only applicable in alkyl carbon atoms number compared with
Few product, increases with carbon atom number in product alkyl, and the yield of product declines, and reaction is incomplete, produces
Thing is difficult to purification.
The content of the invention
The purpose of the present invention is that to solve the above problems and provides a kind of trimethylpyridine-phosphamide chlorine
The method of dihydrocarbon reagent.
The present invention is achieved through the following technical solutions above-mentioned purpose：
The present invention is comprised the following steps：
Step a, in reaction bulb add predetermined amount trimethylpyridine-phosphamide；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca phosphorous acid diamide in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine di-phosphate ester.
Currently preferred, according to step a, the reaction bulb is dry.
Currently preferred, according to step c, in the reaction bulb, Deca phosphorous acid diamide includes：
The Deca phosphorous acid diamide while stirring in the reaction bulb, after completion of dropping, continues stirring, directly
Terminate to reaction.
It is currently preferred, concentration is carried out to the product, after obtaining chlorine di-phosphate ester, the side
Method also includes：
The chlorine di-phosphate ester product is distilled.
Currently preferred, the molal quantity of the predetermined amount trimethylpyridine-phosphamide is higher than the phosphorous acyl two
Amine.
Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 50 70%；The Asia
Composition proportion shared by phosphoryl diamine is 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 60%；The phosphorous acyl
Composition proportion shared by diamidogen is 20%；Composition proportion shared by the anhydrous solvent is 20%.
The beneficial effects of the present invention is：
The present invention does not use any solvent in the preparation process by chlorine phosphate ester, and reaction can be made to carry out completely,
Response time is short, and will not product fluid garbage.Generally products therefrom has sufficiently high purity,
Meet the needs of general organic synthesiss, it is such as dissatisfied to purity further to distill.
Description of the drawings
Fig. 1 is a kind of method of trimethylpyridine of the present invention-phosphamide chlorine dihydrocarbon reagent
Flow chart.
Specific embodiment
The invention will be further described below：
The present invention is comprised the following steps：
As shown in figure 1, the present invention is comprised the following steps：
Step a, in reaction bulb add predetermined amount trimethylpyridine-phosphamide；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca phosphorous acid diamide in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine di-phosphate ester.
Currently preferred, according to step a, the reaction bulb is dry.
Currently preferred, according to step c, in the reaction bulb, Deca phosphorous acid diamide includes：
The Deca phosphorous acid diamide while stirring in the reaction bulb, after completion of dropping, continues stirring, directly
Terminate to reaction.
It is currently preferred, concentration is carried out to the product, after obtaining chlorine di-phosphate ester, the side
Method also includes：
The chlorine di-phosphate ester product is distilled.
Currently preferred, the molal quantity of the predetermined amount trimethylpyridine-phosphamide is higher than the phosphorous acyl two
Amine.
Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 50 70%；The Asia
Composition proportion shared by phosphoryl diamine is 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
Embodiment one：Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 50%；
Composition proportion shared by the phosphorous acid diamide is 30%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment two：Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 55%；
Composition proportion shared by the phosphorous acid diamide is 25%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment three：Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 60%；
Composition proportion shared by the phosphorous acid diamide is 20%；Composition proportion shared by the anhydrous solvent is 20%.
Example IV：Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 70%；
Composition proportion shared by the phosphorous acid diamide is 10%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment five：Currently preferred, composition proportion shared by the trimethylpyridine-phosphamide is 65%；
Composition proportion shared by the phosphorous acid diamide is 15%；Composition proportion shared by the anhydrous solvent is 20%.
Above-described embodiment is presently preferred embodiments of the present invention, is not the restriction to technical solution of the present invention；
As long as without the technical scheme that creative work can be realized on the basis of above-described embodiment, all should regard
For falling in the rights protection scope of patent of the present invention.
Claims (7)
1. the method for a kind of trimethylpyridine-phosphamide chlorine dihydrocarbon reagent, it is characterised in that：Bag
Include following steps：
Step a, in reaction bulb add predetermined amount trimethylpyridine-phosphamide；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca phosphorous acid diamide in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine oleate.
2. a kind of trimethylpyridine according to claim 1-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：According to step a, the reaction bulb is dry.
3. a kind of trimethylpyridine according to claim 1-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：According to step c, in the reaction bulb, Deca phosphorous acid diamide includes：
The Deca phosphorous acid diamide while stirring in the reaction bulb, after completion of dropping, continues stirring, directly
Terminate to reaction.
4. a kind of trimethylpyridine according to claim 1-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：Concentration is carried out to the product, after obtaining chlorine di-phosphate ester, the side
Method also includes：
The chlorine di-phosphate ester product is distilled.
5. a kind of trimethylpyridine according to claim 1-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：The molal quantity of the predetermined amount trimethylpyridine-phosphamide is higher than the phosphorous acyl two
Amine.
6. a kind of trimethylpyridine according to claim 1-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：Composition proportion shared by the trimethylpyridine-phosphamide is 50 70%；The Asia
Composition proportion shared by phosphoryl diamine is 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
7. a kind of trimethylpyridine according to claim 6-phosphamide chlorine dihydrocarbon reagent
Method, it is characterised in that：Composition proportion shared by the trimethylpyridine-phosphamide is 60%；The phosphorous acyl
Composition proportion shared by diamidogen is 20%；Composition proportion shared by the anhydrous solvent is 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510587629.5A CN106518910A (en) | 2015-09-15 | 2015-09-15 | Method for preparing dialkyl chlorophosphate reagent through trimethylpyridine-phosphamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510587629.5A CN106518910A (en) | 2015-09-15 | 2015-09-15 | Method for preparing dialkyl chlorophosphate reagent through trimethylpyridine-phosphamide |
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|---|---|
| CN106518910A true CN106518910A (en) | 2017-03-22 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063492A (en) * | 1992-01-21 | 1992-08-12 | 青海黎明化工厂 | One chlorine tetramethyl phosphoryl diamine, dichloro-dimethyl phosphamide preparation method |
| EP0739895A1 (en) * | 1995-04-26 | 1996-10-30 | Nippon Chemical Industrial Company Limited | Method of preparing diarylchlorophosphate |
| EP1327635A1 (en) * | 2002-01-06 | 2003-07-16 | Bromine Compounds Ltd. | Preparation of phenylphosphate esters of 4,4'-biphenol |
| CN103554175A (en) * | 2013-10-15 | 2014-02-05 | 西北农林科技大学 | Reagent preparation method |
| CN103788140A (en) * | 2014-01-26 | 2014-05-14 | 江西科技师范大学 | Method for synthesizing nucleoside 5'-beta, gamma methylene and dihalogenated methylene triphosphate |
-
2015
- 2015-09-15 CN CN201510587629.5A patent/CN106518910A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1063492A (en) * | 1992-01-21 | 1992-08-12 | 青海黎明化工厂 | One chlorine tetramethyl phosphoryl diamine, dichloro-dimethyl phosphamide preparation method |
| EP0739895A1 (en) * | 1995-04-26 | 1996-10-30 | Nippon Chemical Industrial Company Limited | Method of preparing diarylchlorophosphate |
| EP1327635A1 (en) * | 2002-01-06 | 2003-07-16 | Bromine Compounds Ltd. | Preparation of phenylphosphate esters of 4,4'-biphenol |
| CN103554175A (en) * | 2013-10-15 | 2014-02-05 | 西北农林科技大学 | Reagent preparation method |
| CN103788140A (en) * | 2014-01-26 | 2014-05-14 | 江西科技师范大学 | Method for synthesizing nucleoside 5'-beta, gamma methylene and dihalogenated methylene triphosphate |
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