CN102020571A - Preparation method of tetramethylammonium bromide - Google Patents
Preparation method of tetramethylammonium bromide Download PDFInfo
- Publication number
- CN102020571A CN102020571A CN2009100705389A CN200910070538A CN102020571A CN 102020571 A CN102020571 A CN 102020571A CN 2009100705389 A CN2009100705389 A CN 2009100705389A CN 200910070538 A CN200910070538 A CN 200910070538A CN 102020571 A CN102020571 A CN 102020571A
- Authority
- CN
- China
- Prior art keywords
- bromide
- monobromethane
- gained
- ethyl acetate
- preparation
- 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.)
- Pending
Links
Abstract
The invention relates to a preparation method of tetramethylammonium bromide. The preparation method is characterized by comprising the following steps of: (1) performing a synthetic reaction on the tetramethylammonium bromide; (2) filtering; and (3) refining. The preparation method increases product yield, meets the market demand and enhances the economic and social benefits of an enterprise.
Description
Technical field
The present invention relates to organic compound preparation method field, particularly a kind of preparation method of 4 bromide.
Background technology
4 bromide is a chemical products common on a kind of market, is a kind of ion pair reagent, and polarographic analysis reagent also is a kind of effective phase-transfer catalyst.At present, do not increasing sophisticated equipment and do not strengthening under the situation of operator's technical requirements, the product yield that synthesizes is not high.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of 4 bromide is provided.
The present invention for achieving the above object, by the following technical solutions:
(1) 4 bromide building-up reactions
Monobromethane is added in the etoh solvent, and monobromethane and alcoholic acid ratio of weight and number are 1: 1-1.5, and the ratio of weight and number that stirs and slowly feed Trimethylamine 99, Trimethylamine 99 and monobromethane is 2: 1, does not separate out reaction terminating to there being precipitation;
(2) filter
With the mixture filtration under diminished pressure of reaction back gained, the faint yellow solid of gained is the 4 bromide crude product;
(3) refining
In the 4 bromide crude product, add ethyl acetate, monobromethane ratio of weight and number in ethyl acetate and the step (1) is 1.5: 2, be heated to backflow and be incubated 0.5 hour, crystallisation by cooling then, filter, and product removed remaining ethyl acetate 50 ℃ of decompressions, the white crystal of gained is the 4 bromide finished product.
Among the present invention, described Trimethylamine 99, monobromethane, etoh solvent are the general industry product.
Among the present invention, described reactor has the reactor of heating unit, electric stirring, thermometer, water circulation condenser.
The beneficial effect that the present invention had:
The present invention has improved product yield, has satisfied the demand in market, has improved economic benefit of enterprises and social benefit.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment one:
(1) 4 bromide building-up reactions
In a reactor of 1000 milliliters that has heating unit, electric stirring, thermometer, a water circulation condenser, drop into 200 gram monobromethanes, 200 gram etoh solvents, stir and slowly feed 400 gram Trimethylamine 99s, do not separate out reaction terminating to there being precipitation;
(2) filter
With the mixture filtration under diminished pressure of reaction back gained, the faint yellow solid of gained is the 4 bromide crude product;
(3) refining
In the 4 bromide crude product, add 150 gram ethyl acetate, be heated to backflow and be incubated 0.5 hour, then crystallisation by cooling, filter, and with product 50 ℃ of decompressions, vacuum tightness remains on the 30-35mmHg post, remove remaining ethyl acetate, the white crystal of gained is the 4 bromide finished product.
Embodiment two:
(1) 4 bromide building-up reactions
In a reactor of 1000 milliliters that has heating unit, electric stirring, thermometer, a water circulation condenser, drop into 200 gram monobromethanes, 250 grams ethanol as solvent, stir and slowly feed 400 gram Trimethylamine 99s, do not separate out reaction terminating to there being precipitation;
(2) filter
With the mixture filtration under diminished pressure of reaction back gained, the faint yellow solid of gained is the 4 bromide crude product;
(3) refining
In the 4 bromide crude product, add 150 gram ethyl acetate, be heated to backflow and be incubated 0.5 hour, then crystallisation by cooling, filter, and with product 50 ℃ of decompressions, vacuum tightness remains on the 30-35mmHg post, remove remaining ethyl acetate, the white crystal of gained is the 4 bromide finished product.
Embodiment three:
(1) 4 bromide building-up reactions
In a reactor of 1000 milliliters that has heating unit, electric stirring, thermometer, a water circulation condenser, drop into 200 gram monobromethanes, 300 grams ethanol as solvent, stir and slowly feed 400 gram Trimethylamine 99s, do not separate out reaction terminating to there being precipitation;
(2) filter
With the mixture filtration under diminished pressure of reaction back gained, the faint yellow solid of gained is the 4 bromide crude product;
(3) refining
In the 4 bromide crude product, add 150 gram ethyl acetate, be heated to backflow and be incubated 0.5 hour, then crystallisation by cooling, filter, and with product 50 ℃ of decompressions, vacuum tightness remains on the 30-35mmHg post, remove remaining ethyl acetate, the white crystal of gained is the 4 bromide finished product.
The above only is preferred embodiment of the present invention, is not technical scheme of the present invention is done any pro forma restriction.Every foundation technical spirit of the present invention all still belongs in the scope of technical scheme of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (1)
1. the preparation method of a 4 bromide is characterized in that comprising:
(1) 4 bromide building-up reactions
Monobromethane is added in the etoh solvent, and monobromethane and alcoholic acid ratio of weight and number are 1: 1-1.5, and stir also and slowly feed Trimethylamine 99, the ratio of weight and number of Trimethylamine 99 and monobromethane is 2: 1, does not separate out reaction terminating to there being precipitation;
(2) filter
With the mixture filtration under diminished pressure of reaction back gained, the faint yellow solid of gained is the 4 bromide crude product;
(3) refining
In the 4 bromide crude product, add ethyl acetate, monobromethane ratio of weight and number in ethyl acetate and the step (1) is 1.5: 2, be heated to backflow and be incubated 0.5 hour, crystallisation by cooling then, filter, and product removed remaining ethyl acetate 50 ℃ of decompressions, the white crystal of gained is the 4 bromide finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100705389A CN102020571A (en) | 2009-09-23 | 2009-09-23 | Preparation method of tetramethylammonium bromide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100705389A CN102020571A (en) | 2009-09-23 | 2009-09-23 | Preparation method of tetramethylammonium bromide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102020571A true CN102020571A (en) | 2011-04-20 |
Family
ID=43862393
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100705389A Pending CN102020571A (en) | 2009-09-23 | 2009-09-23 | Preparation method of tetramethylammonium bromide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102020571A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237410A (en) * | 2015-10-26 | 2016-01-13 | 曹仪山 | Method for preparing tetramethyl ammonium bromide |
| CN106187832A (en) * | 2016-07-15 | 2016-12-07 | 北京百灵威科技有限公司 | A kind of method prepared or purify ion-pairing agent |
| CN113443994A (en) * | 2021-06-11 | 2021-09-28 | 上海交通大学 | Organic luminescent material and preparation method and application thereof |
-
2009
- 2009-09-23 CN CN2009100705389A patent/CN102020571A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237410A (en) * | 2015-10-26 | 2016-01-13 | 曹仪山 | Method for preparing tetramethyl ammonium bromide |
| CN105237410B (en) * | 2015-10-26 | 2017-08-01 | 曹仪山 | A kind of method for preparing 4 bromide |
| CN106187832A (en) * | 2016-07-15 | 2016-12-07 | 北京百灵威科技有限公司 | A kind of method prepared or purify ion-pairing agent |
| CN106187832B (en) * | 2016-07-15 | 2018-06-26 | 北京百灵威科技有限公司 | A kind of method for preparing or purifying ion-pairing agent |
| CN113443994A (en) * | 2021-06-11 | 2021-09-28 | 上海交通大学 | Organic luminescent material and preparation method and application thereof |
| CN113443994B (en) * | 2021-06-11 | 2022-10-21 | 上海交通大学 | Organic luminescent material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102020572A (en) | Method for preparing tetrabutyl ammonium bromide | |
| CN101851151A (en) | Method for preparing cyclohexanol by using cyclohexene | |
| CN102976917A (en) | Aqueous-phase refining method of long-chain dibasic acid | |
| CN102020571A (en) | Preparation method of tetramethylammonium bromide | |
| CN103012114B (en) | Method of synchronously preparing DL-tartaric acid and DL-potassium hydrogen tartrate | |
| CN101157615A (en) | Method for producing plasticizer phthalic acid dinonyl | |
| CN102250969B (en) | Process for preparing high-purity resveratrol from giant knotweed | |
| CN102786403B (en) | Preparation method for 4-tertiary butyl-4'-methoxy dibenzoyl methane | |
| CN102020569A (en) | Method for preparing tetraethyl ammonium bromide | |
| CN105175276A (en) | Synthetic method for optically pure(R)-3-carbamyl methyl-5-methyl caproic acid | |
| CN102020570A (en) | Preparation method for tetrapropyl ammonium bromide | |
| CN103588336B (en) | Method for utilizing low-concentration acetic acid wastewater | |
| CN103524402A (en) | Preparation method of efficient stable inhibitor | |
| CN102500397B (en) | Preparation method for solid super acid catalyst for synthesis of levulinic acid and application of solid super acid catalyst | |
| CN108004351B (en) | Refining method of xylose hydrolysate | |
| CN102504958B (en) | Method for separating unsaturated fatty acids from silkworm chrysalis oil based on composition complexation of reversible reaction | |
| CN102040527A (en) | Preparation method of N,N-benzyl diphenylamine | |
| CN101914015B (en) | Preparation and purification method of butyl stearate | |
| CN103420882A (en) | Method for preparing L-methionine | |
| CN106518666A (en) | Preparation method for refining dibutyl adipate | |
| CN102924961A (en) | Preparation method for disperse red | |
| CN105272853A (en) | Preparation method for diisooctyl adipate | |
| CN107163099A (en) | A kind of (18 β, 20 β) 24 hydroxyl radix glycyrrhizae acid esters and preparation method thereof | |
| CN106518667A (en) | Method for refining di-n-butyl adipate | |
| CN101811972A (en) | Method for separating and purifying 2-chlorine-4,6-dinitroresorcinol in dilution crystallization method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110420 |