CN103539629A - Preparation method of 1, 4-dibromo-2-butene - Google Patents
Preparation method of 1, 4-dibromo-2-butene Download PDFInfo
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- CN103539629A CN103539629A CN201210246370.4A CN201210246370A CN103539629A CN 103539629 A CN103539629 A CN 103539629A CN 201210246370 A CN201210246370 A CN 201210246370A CN 103539629 A CN103539629 A CN 103539629A
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- bromo
- butylene
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- butadiene
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a preparation method of 1, 4-dibromo-2-butene. The method comprises the following steps: adding chloroform into a reactor, and decreasing the temperature to be less than -10 DEG C; filling 1, 3-butadiene through a gas-guide tube, stirring and decreasing the temperature to be below -15 DEG C; then dripping bromine, controlling the temperature to be -15 DEG C, and distilling the chloroform and the unreacted 1, 3-butadiene at reduced pressure after finishing the dripping; and adding petroleum ether to recrystallize after completing the distilling, filtering to obtain a solid product, and carrying out vacuum drying so as to obtain the 1, 4-dibromo-2-butene. The method is simple to operate and low in cost, causes less pollution, and is high in product purity and suitable for industrial large-scale application.
Description
Technical field
The present invention relates to a kind of preparation method of bromo alkene, specifically relate to the preparation method of the bromo-2-butylene of a kind of Isosorbide-5-Nitrae-bis-.
Background technology
The bromo-2-butylene of Isosorbide-5-Nitrae-bis-is a kind of medicine intermediate, and it carries out the exploitation of bulk drug as raw material take at present more producer both at home and abroad, has good market outlook.The synthetic method of the bromo-2-butylene of Isosorbide-5-Nitrae-bis-of the prior art exists the defect that reaction yield is low, product purity is low.
Summary of the invention
For the shortcoming and defect of prior art existence, the invention provides the preparation method of the bromo-2-butylene of a kind of Isosorbide-5-Nitrae-bis-, the present invention is simple to operate, and cost is low, pollutes less, is suitable for industrial large-scale application.
The present invention is achieved through the following technical solutions:
A preparation method for the bromo-2-butylene of Isosorbide-5-Nitrae-bis-, described preparation method comprises the following steps:
Step (1) adds chloroform in reactor, cools to below-10 ℃;
Step (2) passes into 1,3-butadiene with airway in described reactor, stirs and cools to below-15 ℃;
Step (3) drips bromine in described reactor, controls temperature-15 ℃;
Step (4), after dropping bromine finishes, underpressure distillation goes out chloroform and unreacted 1,3-butadiene;
Step (5), after distillation finishes, adds sherwood oil recrystallization, filters and obtains solid phase prod, and vacuum-drying, obtains.
Preferably, the chloroform in described step (1) is 6 weight parts.
Preferably, the 1,3-butadiene passing into airway in described step (2) is 1 weight part.
Preferably, the bromine dripping in described step (3) is 2.4 weight parts.
Preferably, described step (5) PetroChina Company Limited. ether is 2.2 weight parts.
The present invention is simple to operate, and cost is low, pollutes less, is suitable for industrial large-scale application.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of preparing the bromo-2-butylene of Isosorbide-5-Nitrae-bis-.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
A preparation method for the bromo-2-butylene of Isosorbide-5-Nitrae-bis-, comprises the following steps (as shown in Figure 1):
(1) will in reactor, add the chloroform of 6 weight parts, cool to below-10 ℃;
(2) with airway to the 1,3-butadiene that passes into 1 weight part in described reactor, stir and cool to below-15 ℃;
(3) then to the bromine that drips 2.4 weight parts in described reactor, control temperature-15 ℃;
(4) after dropping finishes, underpressure distillation goes out chloroform and unreacted 1,3-butadiene;
(5) after distillation finishes, add the sherwood oil recrystallization of 2.2 weight parts, filter and obtain solid phase prod, vacuum-drying, obtains.
Claims (5)
1. a preparation method for 4-bis-bromo-2-butylene, is characterized in that: described preparation method comprises the following steps:
Step (1) adds chloroform in reactor, cools to below-10 ℃;
Step (2) passes into 1,3-butadiene with airway in described reactor, stirs and cools to below-15 ℃;
Step (3) drips bromine in described reactor, controls temperature-15 ℃;
Step (4), after dropping bromine finishes, underpressure distillation goes out chloroform and unreacted 1,3-butadiene;
Step (5), after distillation finishes, adds sherwood oil recrystallization, filters and obtains solid phase prod, and vacuum-drying, obtains.
2. the preparation method of the bromo-2-butylene of Isosorbide-5-Nitrae-bis-according to claim 1, is characterized in that: the chloroform in described step (1) is 6 weight parts.
3. the preparation method of the bromo-2-butylene of Isosorbide-5-Nitrae-bis-according to claim 1, is characterized in that: the 1,3-butadiene passing into airway in described step (2) is 1 weight part.
4. the preparation method of the bromo-2-butylene of Isosorbide-5-Nitrae-bis-according to claim 1, is characterized in that: the bromine dripping in described step (3) is 2.4 weight parts.
5. according to the preparation method of the bromo-2-butylene of Isosorbide-5-Nitrae-bis-described in claim 1 to 4 any one, it is characterized in that: described step (5) PetroChina Company Limited. ether is 2.2 weight parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210246370.4A CN103539629A (en) | 2012-07-17 | 2012-07-17 | Preparation method of 1, 4-dibromo-2-butene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210246370.4A CN103539629A (en) | 2012-07-17 | 2012-07-17 | Preparation method of 1, 4-dibromo-2-butene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103539629A true CN103539629A (en) | 2014-01-29 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210246370.4A Pending CN103539629A (en) | 2012-07-17 | 2012-07-17 | Preparation method of 1, 4-dibromo-2-butene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103539629A (en) |
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2012
- 2012-07-17 CN CN201210246370.4A patent/CN103539629A/en active Pending
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| PB01 | Publication | ||
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Application publication date: 20140129 |