CN101824026A - New synthesis method of trithio spices - Google Patents
New synthesis method of trithio spices Download PDFInfo
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- CN101824026A CN101824026A CN201010148828A CN201010148828A CN101824026A CN 101824026 A CN101824026 A CN 101824026A CN 201010148828 A CN201010148828 A CN 201010148828A CN 201010148828 A CN201010148828 A CN 201010148828A CN 101824026 A CN101824026 A CN 101824026A
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- trithio
- dimethyl
- sulphur
- divinyl
- spices
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Abstract
The invention provides a simple method for synthesizing 3,5-dimethyl-1,2,4-trithio cyclopentane compounds.
Description
Technical field
The invention belongs to the chemical industry field of perfumery, for novel 3,5-dimethyl-1,2, the high efficiency preparation method of 4-trithio pentamethylene.
3,5-dimethyl-1,2,4-trithio cyclopentane structure formula
Background technology
Novel fragrance 3,5-dimethyl-1,2,4-trithio pentamethylene preparation difficulty, the synthetic method of bibliographical information seldom, HelveticaChimica Acta wherein, vol.61, Fasc.4 (1978)-Nr.140 has reported that with α-chloroethyl sulfur subchloride be raw material, with in the dimethyl formamide with sodium sulphite reaction, generate product, this method raw material is difficult to obtain, and yield is low, and purity is not high; Document has reported with acetaldehyde to be raw material again, reaction in the presence of sulphur and sodium sulphite, but this method yield only 5%, and product is difficult to purify from a pile impurity, no actual production meaning.
A purpose of the present invention is in order to provide a kind of preparation simple and convenient preparation high purity 3,5-dimethyl-1,2, and the method for 4-trithio pentamethylene solves the yield in the preparation and the purity problem of product, and suitability for industrialized production is achieved.
Technical scheme of the present invention
We are surprised to find under study for action accidentally, and dialkylene two sulphur can be easy to reaction with hydrogen sulfide and produce 3,5-dimethyl-1,2, and 4-trithio pentamethylene, yield height, and reaction conditions gentleness, raw material is easy to get, and the product purity height satisfies eating requirements fully.
Through more careful research, we find that reaction can have solvent or solvent-free, optional polar solvent of solvent or non-polar solvent, and hydrogen sulfide can directly be ventilated, or directly produces use, uses as generating under acidic conditions directly with sulfide.
Specific embodiment
Embodiment 1
Under nitrogen protection, divinyl two sulphur 100 grams are added in the 1000ml there-necked flask, add the 500ml anhydrous methanol; stir; it is extremely saturated slowly to lead to hydrogen sulfide down at 0 ℃, is stirred to react completely, and is spin-dried for; directly rectification under vacuum; collect 75～80 ℃ of fractions and promptly get product, be 3,5-dimethyl-1; 2,4-trithio pentamethylene.
Embodiment 2
Under nitrogen protection, divinyl two sulphur 100 grams are added in the 1000ml there-necked flask, add the 500ml dehydrated alcohol; stir; it is extremely saturated slowly to lead to hydrogen sulfide down at 0 ℃, is stirred to react completely, and is spin-dried for; directly rectification under vacuum; collect 75～80 ℃ of fractions and promptly get product, be 3,5-dimethyl-1; 2,4-trithio pentamethylene.
Embodiment 3
Under nitrogen protection, divinyl two sulphur 100 grams are added in the 1000ml there-necked flask, add the 500ml dimethyl formamide; stir; it is extremely saturated slowly to lead to hydrogen sulfide down at 0 ℃, is stirred to react completely, and is spin-dried for; directly rectification under vacuum; collect 75～80 ℃ of fractions and promptly get product, be 3,5-dimethyl-1; 2,4-trithio pentamethylene.
Embodiment 4
Under nitrogen protection, divinyl two sulphur 100 grams are added in the 1000ml there-necked flask, add the 500ml anhydrous methanol; stir, add nine hydrated sodium sulfides, 100 grams, slowly dripping hydrochloric acid 50ml down at 0 ℃; be stirred to and react completely; be spin-dried for, directly rectification under vacuum is collected 75～80 ℃ of fractions and is promptly got product; be 3; 5-dimethyl-1,2,4-trithio pentamethylene.
Claims (3)
1. one kind 3,5-dimethyl-1,2, the synthetic method of 4-trithio pentamethylene is characterized in that with divinyl two sulphur be starting raw material.
2. according to claim 1, it is characterized in that with divinyl two sulphur be starting raw material, divinyl two sulphur and hydrogen sulfide generation addition reaction generation obtained, can be shown below:
3. shown in claim 2, hydrogen sulfide can use by producing directly in the reaction, generates as add acid with sodium sulphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010148828A CN101824026A (en) | 2010-04-19 | 2010-04-19 | New synthesis method of trithio spices |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010148828A CN101824026A (en) | 2010-04-19 | 2010-04-19 | New synthesis method of trithio spices |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101824026A true CN101824026A (en) | 2010-09-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010148828A Pending CN101824026A (en) | 2010-04-19 | 2010-04-19 | New synthesis method of trithio spices |
Country Status (1)
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| CN (1) | CN101824026A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837554A (en) * | 2016-05-06 | 2016-08-10 | 河北科技大学 | Synthesis method for 1,3,5-trithio heterocyclic hexane derivative |
-
2010
- 2010-04-19 CN CN201010148828A patent/CN101824026A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837554A (en) * | 2016-05-06 | 2016-08-10 | 河北科技大学 | Synthesis method for 1,3,5-trithio heterocyclic hexane derivative |
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| 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: 20100908 |