CN101885669A - Preparation method of 4-vinyl guaiacol - Google Patents
Preparation method of 4-vinyl guaiacol Download PDFInfo
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- CN101885669A CN101885669A CN201010229531XA CN201010229531A CN101885669A CN 101885669 A CN101885669 A CN 101885669A CN 201010229531X A CN201010229531X A CN 201010229531XA CN 201010229531 A CN201010229531 A CN 201010229531A CN 101885669 A CN101885669 A CN 101885669A
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Abstract
The invention relates to a preparation method of 4-vinyl guaiacol, which comprises the following steps: (1) putting quinoline, ferulic acid and hydroquinone as a polymerization inhibitor in a reactor in sequence, opening a heating device, switching on a nitrogen protection device, stopping heating until no air overflows from a system, and then continuing to stir for 40-60min; (2) adding phene in the reaction and evenly stirring, adding hydrochloric acid in the solution, stirring evenly, then standing for layering until the aqueous phase pH value is detected to be neutral, and then finally adding desiccating agent anhydrous calcium chloride in the solution washed with deionized water; and (3) putting the dried solution in a distiller, steaming the benzene as the solvent out, then connecting to a vacuum pump, steaming out the product at the gas phase temperature below 100 DEG C, and packing for sale. The invention carries out comparation research on the synthesis process of the 4-vinyl guaiacol, and determines the optimum reaction matching of the various reactants of ferulic acid and quinoline, thereby improving the reaction yield, and enabling the 4-vinyl guaiacol to be more suitable for the requirement of the industrial production.
Description
Technical field
The invention belongs to the organic compound preparation field, especially a kind of preparation method of spices 4-vinyl guaiacol.
Background technology
The 4-vinyl guaiacol is a kind of flavouring agent, has unique toast earthnut meat flavour, be mainly used in the interpolation of the fragrant composition of drinks, also be used for industries such as cigarette, food, daily use chemicals, medical essence be synthetic simultaneously, and can be used for the allotment of apple, spice, sootiness essence.
But existing processes is comparatively complicated, and yield is lower.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the preparation method of the 4-vinyl guaiacol that a kind of technology is simple, yield is higher is provided.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of 4-vinyl guaiacol, preparation method's step is:
(1) reaction: in a reactor that has heating unit, electric stirring, thermometer, water circulation condenser and a nitrogen protection device, drop into quinoline, forulic acid successively and as the Resorcinol of stopper, open heating unit, connect nitrogen protection device, when system temperature is elevated to 180-185 degree centigrade, have bubble from system, to overflow, accelerate stirring velocity immediately this moment, so reaction is about 4-5 hour, does not have gas to system and overflows and stop heating, continues stirring 40-60 minute;
(2) wash material: with above-mentioned reaction solution standing over night, in reaction solution, stir in the adding solvent benzol then, and in this solution, add hydrochloric acid, stir, standing demix then, discard water layer, so repeat at least three times, and then in the solution after the salt pickling, add deionized water, stir, standing demix discards water layer then, detects ph value of aqueous phase and is till the neutrality; Add the siccative Calcium Chloride Powder Anhydrous in the solution after the deionization washing at last;
(3) refining: dried solution is put into distiller, and normal pressure will steam as the benzene of solvent, connects last vacuum pump then and under the gas phase temperature below 100 degrees centigrade product is steamed, and can pack commercially available.
And described quinoline: the ratio of weight and number of forulic acid is 2-2.4: 1.
And described vacuum pump is the low-pressure vacuum pump of 3-5 mmhg vacuum tightness.
Advantage of the present invention and beneficial effect are:
The present invention has determined various reactant forulic acid by research that the synthesis technique of 4-vinyl guaiacol is compared, the optimum response proportioning of quinoline.Therefore reaction yield is improved, and make it more appropriate to industrial requirement.
Embodiment
The invention will be further described below by specific embodiment.Following examples are descriptive, are not restrictive, can not limit protection scope of the present invention with this.
Embodiment 1:
A kind of preparation method of 4-vinyl guaiacol, the step of preparation is:
(1) reaction: in a reactor of 1000 milliliters that has heating unit, electric stirring, thermometer, water circulation condenser and a nitrogen protection device, drop into 500 milliliters of quinoline, 250 gram forulic acid successively and as the Resorcinol of stopper; Open heating unit and will heat regulating and controlling to 250 degree centigrade, connect nitrogen protection device then and slowly feed nitrogen; When system temperature is elevated to 180-185 degree centigrade, there is bubble from system, to overflow, accelerate stirring velocity immediately this moment, so react about 4-5 hour, do not have gas to system and overflow and stop heating, continue to stir 40-60 minute;
(2) wash material: with the reaction solution standing over night, and add in reaction solution in 2000 milliliters the benzene and stir, add 500 milliliters of 30% hydrochloric acid then in this solution, stir, standing demix discards water layer then, so repeats at least three times; And then in the solution after the salt pickling, add deionized water, and stirring, standing demix discards water layer then, detects ph value of aqueous phase and is till the neutrality; Add the siccative Calcium Chloride Powder Anhydrous in the solution after the deionization washing at last;
(3) refining: as will to put into distiller in the dried solution, normal pressure will steam as the benzene of solvent, connects then and goes up vacuum unit, and the vacuum pump that uses is the low-pressure vacuum pump of 3-5 mmhg vacuum tightness, under the gas phase temperature below 100 degrees centigrade, product is steamed, can pack commercially available.
Quinoline involved in the present invention, forulic acid and be the general industry product as the Resorcinol of stopper.
Embodiment 2:
A kind of preparation method of 4-vinyl guaiacol, the step of preparation is:
(1) reaction: have heating unit to one, electricity stirs, thermometer, in 1000 milliliters the reactor of water circulation condenser and nitrogen protection device, drop into 550 milliliters of quinoline successively, 250 gram forulic acid and as the Resorcinol of stopper, open heating unit and will heat regulating and controlling to 250 degree centigrade, connect nitrogen protection device then and slowly feed nitrogen, when system temperature is elevated to 180-185 degree centigrade, there is bubble from system, to overflow, accelerate stirring velocity immediately this moment, so reaction is about 4-5 hour, do not have gas to system and overflow and stop heating, continue to stir 40-60 minute;
(2) wash material: with the reaction solution standing over night, add in reaction solution then in 2000 milliliters the benzene and stir, add 500 milliliters of 30% hydrochloric acid in this solution, stir, standing demix discards water layer then, so repeats at least three times; And then in the solution after the salt pickling, add deionized water, and stirring, standing demix discards water layer then, detects ph value of aqueous phase and is till the neutrality; Add the siccative Calcium Chloride Powder Anhydrous in the solution after the deionization washing at last;
(3) refining: that dried solution is put into distiller, normal pressure will steam as the benzene of solvent, connects then and goes up vacuum unit, and the vacuum pump that uses is the low-pressure vacuum pump of 3-5 mmhg vacuum tightness, under the gas phase temperature below 100 degrees centigrade, product is steamed, can pack commercially available.
Embodiment 3:
A kind of preparation method of 4-vinyl guaiacol, the step of preparation is:
(1) reaction: have heating unit to one, electricity stirs, thermometer, in 1000 milliliters the reactor of water circulation condenser and nitrogen protection device, drop into 600 milliliters of quinoline successively, 250 gram forulic acid and as the Resorcinol of stopper, open heating unit and will heat regulating and controlling to 250 degree centigrade, connect nitrogen protection device then and slowly feed nitrogen, when system temperature is elevated to 180-185 degree centigrade, there is bubble from system, to overflow, accelerate stirring velocity immediately this moment, so reaction is about 4-5 hour, do not have gas to system and overflow and stop heating, continue to stir 40-60 minute;
(2) wash material: with the reaction solution standing over night, add in reaction solution then in 2000 milliliters the benzene and stir, add 500 milliliters of 30% hydrochloric acid in this solution, stir, standing demix discards water layer then, so repeats at least three times; And then in the solution after the salt pickling, add deionized water, and stirring, standing demix discards water layer then, detects ph value of aqueous phase and is till the neutrality; Add the siccative Calcium Chloride Powder Anhydrous in the solution after the deionization washing at last.
(3) refining: that dried solution is put into distiller, normal pressure will steam as the benzene of solvent, connects then and goes up vacuum unit, and the vacuum pump that uses is the low-pressure vacuum pump of 3-5 mmhg vacuum tightness, under the gas phase temperature below 100 degrees centigrade, product is steamed, can pack commercially available.
Claims (3)
1. the preparation method of a 4-vinyl guaiacol, it is characterized in that: preparation method's step is:
(1) reaction: in a reactor that has heating unit, electric stirring, thermometer, water circulation condenser and a nitrogen protection device, drop into quinoline, forulic acid successively and as the Resorcinol of stopper, open heating unit, connect nitrogen protection device, when system temperature is elevated to 180-185 degree centigrade, have bubble from system, to overflow, accelerate stirring velocity immediately this moment, so reaction is about 4-5 hour, does not have gas to system and overflows and stop heating, continues stirring 40-60 minute;
(2) wash material: with above-mentioned reaction solution standing over night, in reaction solution, stir in the adding solvent benzol then, and in this solution, add hydrochloric acid, stir, standing demix then, discard water layer, so repeat at least three times, and then in the solution after the salt pickling, add deionized water, stir, standing demix discards water layer then, detects ph value of aqueous phase and is till the neutrality; Add the siccative Calcium Chloride Powder Anhydrous in the solution after the deionization washing at last;
(3) refining: dried solution is put into distiller, and normal pressure will steam as the benzene of solvent, connects last vacuum pump then and under the gas phase temperature below 100 degrees centigrade product is steamed, and can pack commercially available.
2. 4-vinyl guaiacol according to claim 1 is characterized in that: described quinoline: the ratio of weight and number of forulic acid is 2-2.4: 1.
3. 4-vinyl guaiacol according to claim 1 is characterized in that: described vacuum pump is the low-pressure vacuum pump of 3-5 mmhg vacuum tightness.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010229531XA CN101885669A (en) | 2010-07-17 | 2010-07-17 | Preparation method of 4-vinyl guaiacol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010229531XA CN101885669A (en) | 2010-07-17 | 2010-07-17 | Preparation method of 4-vinyl guaiacol |
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| CN201010229531XA Pending CN101885669A (en) | 2010-07-17 | 2010-07-17 | Preparation method of 4-vinyl guaiacol |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776246A (en) * | 2012-08-15 | 2012-11-14 | 山东省科学院能源研究所 | Mehtod for preparing natural 4-vinyl guaiacol by biological transformation |
| CN102899212A (en) * | 2012-11-08 | 2013-01-30 | 山东轻工业学院 | Method for increasing content of 4-vinyl guaiacol in top fermentation wheat beer |
| CN104496768A (en) * | 2014-11-20 | 2015-04-08 | 中国农业科学院油料作物研究所 | Highly-efficient synthetic method for 2, 6-dimethoxy-4-vinylphenol |
| CN105002225A (en) * | 2015-09-02 | 2015-10-28 | 常州市长宇实用气体有限公司 | Method for preparing 4-ethenyl guaiacol by utilizing bagasse |
| CN113291016A (en) * | 2021-04-30 | 2021-08-24 | 江苏金格润科技有限公司 | Special packaging film of ultra-thin BOPP cigarette |
-
2010
- 2010-07-17 CN CN201010229531XA patent/CN101885669A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776246A (en) * | 2012-08-15 | 2012-11-14 | 山东省科学院能源研究所 | Mehtod for preparing natural 4-vinyl guaiacol by biological transformation |
| CN102899212A (en) * | 2012-11-08 | 2013-01-30 | 山东轻工业学院 | Method for increasing content of 4-vinyl guaiacol in top fermentation wheat beer |
| CN104496768A (en) * | 2014-11-20 | 2015-04-08 | 中国农业科学院油料作物研究所 | Highly-efficient synthetic method for 2, 6-dimethoxy-4-vinylphenol |
| CN105002225A (en) * | 2015-09-02 | 2015-10-28 | 常州市长宇实用气体有限公司 | Method for preparing 4-ethenyl guaiacol by utilizing bagasse |
| CN113291016A (en) * | 2021-04-30 | 2021-08-24 | 江苏金格润科技有限公司 | Special packaging film of ultra-thin BOPP cigarette |
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Application publication date: 20101117 |
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