CN103553890A - Synthesis method of 4-chloro-2-butanone - Google Patents
Synthesis method of 4-chloro-2-butanone Download PDFInfo
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- CN103553890A CN103553890A CN201310512332.3A CN201310512332A CN103553890A CN 103553890 A CN103553890 A CN 103553890A CN 201310512332 A CN201310512332 A CN 201310512332A CN 103553890 A CN103553890 A CN 103553890A
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- butanone
- chloro
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- room temperature
- synthetic method
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/63—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a synthesis method of 4-chloro-2-butanone. The method comprises the following steps: adding a 4-hydroxyl-2-butanone solution in a four-neck bottle of 500 ml and cooling to 5 DEG C below zero; dropwise adding a thionyl chloride solution into the four-neck bottle, preserving the heat for 2-3 hours at the room temperature after the thionyl chloride solution is dropwise added, heating to 60 DEG C and preserving the heat for 0.5-1 hour, and then cooling to the room temperature; washing the solution of the previous step by using 5wt% sodium bicarbonate until the pH (potential of Hydrogen) value is 7 and then decompressing to obtain the 4-chloro-2-butanone product. According to the method, the synthesis yield can be further improved while the use of the solvent is reduced, the technological conditions are simple and convenient, fewer pieces of chemical equipment are used, the flow is short, and the synthesis method is suitable for industrial production and thus has broad market space.
Description
Technical field
The invention belongs to chemical industry preparing technical field, be specifically related to the chloro-2-butanone synthetic method of a kind of 4-.
Background technology
The chloro-2-butanone of 4-is a kind of intermediate conventional in organic synthesis, in the synthetic field of many chemical industry, is widely used.The technique of the chloro-2-butanone of existing preparation 4-is synthetic in normal hexane by 4-hydroxy-2-butanone and sulfur oxychloride, and this process recovery ratio is on the low side, and the normal hexane of introduction has certain waste when reclaiming, and is not suitable for suitability for industrialized production.
Summary of the invention
The technical problem to be solved in the present invention is to provide that a kind of processing condition are easy, flow process is short, synthetic ratio is high, is easy to realize the chloro-2-butanone synthetic method of 4-of suitability for industrialized production.
For solving above technical problem, technical scheme of the present invention is: the chloro-2-butanone synthetic method of a kind of 4-, is characterized in that comprising the steps:
(1) in the four-hole bottle of 500ml, add 4-hydroxy-2-butanone solution, be cooled to-5 ℃;
(2) in four-hole bottle, drip sulfur oxychloride solution, drip and finish rear room temperature insulation 2～3 hours, be warming up to 60 ℃ of insulations after 0.5～1 hour, be cooled to room temperature;
(3) by the upper pH value to 7 that walks solution of sodium hydrogen carbonate solution washing of 5wt%, then decompression obtains the chloro-2-butanone goods of 4-.
The add-on of described 4-hydroxy-2-butanone solution is 50g.
The add-on of described sulfur oxychloride is 82g.
The chloro-2-butanone goods of described 4-synthetic ratio is more than 95%.
Innovation of the present invention is not use normal hexane solvent in building-up process, improves holding temperature simultaneously, makes to react carry out more thorough, and can suitably reduce synthesis temperature, operates convenient.Processing condition of the present invention are easy, and the chemical industry equipment of use is few, flow process is short, is applicable to suitability for industrialized production, therefore possess the potentiality that good market outlook and industry are amplified.
Embodiment
Below in conjunction with embodiment, the present invention is further detailed explanation.
Embodiment 1
The first step: add 50g4-hydroxy-2-butanone solution in the four-hole bottle of 500ml, be cooled to-5 ℃;
Second step: drip 82g sulfur oxychloride solution in four-hole bottle, drip and finish rear room temperature insulation 2 hours, be warming up to 60 ℃ of insulations after 0.5 hour, be cooled to room temperature;
The 3rd step: by the upper pH value to 7 that walks solution of sodium hydrogen carbonate solution washing of 5wt%, then decompression obtains the chloro-2-butanone goods of 47g4-.
Embodiment 2
The first step: add 50g4-hydroxy-2-butanone solution in the four-hole bottle of 500ml, be cooled to-5 ℃;
Second step: drip 82g sulfur oxychloride solution in four-hole bottle, drip and finish rear room temperature insulation 2.5 hours, be warming up to 60 ℃ of insulations after 0.9 hour, be cooled to room temperature;
The 3rd step: by the upper pH value to 7 that walks solution of sodium hydrogen carbonate solution washing of 5wt%, then decompression obtains the chloro-2-butanone goods of 48g4-.
Claims (4)
1. the chloro-2-butanone synthetic method of 4-, is characterized in that comprising the steps:
(1) in the four-hole bottle of 500ml, add 4-hydroxy-2-butanone solution, be cooled to-5 ℃;
(2) in four-hole bottle, drip sulfur oxychloride solution, drip and finish rear room temperature insulation 2～3 hours, be warming up to 60 ℃ of insulations after 0.5～1 hour, be cooled to room temperature;
(3) with the upper pH value to 7 that walks solution of sodium hydrogen carbonate solution washing of 5wt%, then decompression obtains the chloro-2-butanone goods of 4-.
2. the chloro-2-butanone synthetic method of 4-according to claim 1, is characterized in that: the add-on of described 4-hydroxy-2-butanone solution is 50g.
3. the chloro-2-butanone synthetic method of 4-according to claim 1, is characterized in that: the add-on of described sulfur oxychloride is 82g.
4. the chloro-2-butanone synthetic method of 4-according to claim 1, is characterized in that: the chloro-2-butanone goods of described 4-synthetic ratio is more than 95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310512332.3A CN103553890A (en) | 2013-10-23 | 2013-10-23 | Synthesis method of 4-chloro-2-butanone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310512332.3A CN103553890A (en) | 2013-10-23 | 2013-10-23 | Synthesis method of 4-chloro-2-butanone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103553890A true CN103553890A (en) | 2014-02-05 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310512332.3A Pending CN103553890A (en) | 2013-10-23 | 2013-10-23 | Synthesis method of 4-chloro-2-butanone |
Country Status (1)
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| CN (1) | CN103553890A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746282A (en) * | 2019-11-04 | 2020-02-04 | 天津市安凯特科技发展有限公司 | Synthetic method of 4-chloro-2-butanone |
-
2013
- 2013-10-23 CN CN201310512332.3A patent/CN103553890A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| F.S.MUKHAMETOV ET AL: "Reaction of keto alcohols with organophosphorus compounds communication 7.reaction of β-keto alcohols with phosphorus trichloride", 《IZVESTIYA AKADEMII NAUK SSSR, SERIYA KHIMICHESKAYA》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110746282A (en) * | 2019-11-04 | 2020-02-04 | 天津市安凯特科技发展有限公司 | Synthetic method of 4-chloro-2-butanone |
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Application publication date: 20140205 |