CN102030682A - Preparation method of 4-bromo-2,2-diphenylbutyronitrile - Google Patents
Preparation method of 4-bromo-2,2-diphenylbutyronitrile Download PDFInfo
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- CN102030682A CN102030682A CN2010105664405A CN201010566440A CN102030682A CN 102030682 A CN102030682 A CN 102030682A CN 2010105664405 A CN2010105664405 A CN 2010105664405A CN 201010566440 A CN201010566440 A CN 201010566440A CN 102030682 A CN102030682 A CN 102030682A
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- diphenatril
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- bromotrifluoromethane
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Abstract
The invention relates to a preparation method of 4-bromo-2,2-diphenylbutyronitrile. The process steps are as follows: adding ethylene dibromide into a reaction pot, and adding diphenyl acetonitrile and benzalkonium bromide while stirring; adding 60% alkaline solution prepared from caustic soda flakes slowly into the reaction pot and controlling the temperature inside the pot to be not more than 90 DEG C; after adding the caustic soda flakes, discharging cooling water and stirring for 45-90 minutes; after the temperature inside the pot drops naturally, starting to heat slowly until the temperature is 90-98 DEG C, and preserving the temperature for reaction time for 4-6 hours; after the temperature preserving, cooling until the temperature inside the pot is below 70 DEG C, adding water into the pot and stirring continuously; after crystallization, cooling down to a temperature below 30 DEG C, standing for more than 4 hours, filtering and washing the crystals with water to get neutral crystals; and finally getting the 4-bromo-2,2-diphenylbutyronitrile by drying or baking. In the method provided by the invention, the benzalkonium bromide and sodium hydroxide are utilized as catalysts, thus the reaction rate and the yield are greatly improved.
Description
Technical field
The present invention relates to the preparation method of bromotrifluoromethane diphenatril.
Background technology
Side chain is synthetic in the existing diphenoxylate hydrochloride preparation process, be in bromotrifluoromethane diphenatril synthetic, the synthetic middle catalyzer that adopts of diphenatril and ethylene dibromide is a sodium hydroxide, adopt sodium hydroxide not ideal enough as catalyst reaction efficient, about 24 hours reaction times, the organic reaction overlong time exists may produce the problem of side reaction.
Summary of the invention
In order to overcome above-mentioned defective, the technical problem to be solved in the present invention is: the synthetic middle catalyzer that adopts at existing diphenatril and ethylene dibromide is long problem of sodium hydroxide reaction times, the invention provides a kind of preparation method of bromotrifluoromethane diphenatril, it adopts Morpan BB and sodium hydroxide as catalyzer, has improved speed of reaction and productive rate greatly.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of bromotrifluoromethane diphenatril has following processing step: ethylene dibromide is dropped into reactor, stir and drop into diphenatril and Morpan BB down; To be that 60% alkaline solution slowly adds reactor with the concentration of sheet alkali preparation, temperature be no more than 90 ℃ in the control, finishes, and emits water coolant, stirs 45～90 minutes, after temperature descends voluntarily in treating, begins to heat, and is warming up to 90 ℃～98 ℃ insulation reaction 4～6 hours; Insulation finishes, and temperature is below 70 ℃ in being cooled to, and adds water and goes into reactor, continues to stir, separate out crystallization after, be cooled to below 30 ℃, leave standstill more than 4 hours, filter, wash with water to neutrality, dry or dry, get the bromotrifluoromethane diphenatril.
Can control the insulation reaction temperature better for reaching, after described alkaline solution adds reactor, emit water coolant after, the churning time that before heating up the raw material in the reactor is stirred is 60～70 minutes.
As preferably, after described insulation reaction finished, temperature was 40～55 ℃ in reactor was cooled to.
As preferably, described crystallization is separated out, and temperature was 5～15 ℃ in reactor was cooled to.
As preferably, the quality proportioning that feeds intake of described raw material is:
| Name of material | Proportioning |
| Diphenatril | 1 |
| Ethylene dibromide | 1.25-2 |
| Morpan BB | 0.025-0.06 |
| Sheet alkali | 0.9-1.2 |
The invention has the beneficial effects as follows, the preparation method of bromotrifluoromethane diphenatril of the present invention, adopt Morpan BB and sodium hydroxide as catalyzer, reaction times foreshortened to about ten hours, improve speed of reaction greatly, and compare as catalyzer with original technology sodium hydroxide, original process yield is 85%, productive rate of the present invention reaches 150%, and its productive rate also improves a lot.
Embodiment
To help to understand the present invention by following examples, but not limit content of the present invention.Especially the data among the embodiment do not limit the consumption of each composition in the invention.
Chemical equation of the present invention is as follows:
Embodiment 1: the quality that feeds intake proportioning such as following table:
| Name of material | Proportioning |
| Diphenatril | 1 |
| Ethylene dibromide | 1.45 |
| Morpan BB | 0.025 |
| Sheet alkali | 1.03 |
The concrete processing step of the preparation method of bromotrifluoromethane diphenatril of the present invention is:
Confirm reactor drying, cleaning, shut the reactor bottom valve, prepare to feed intake.The ethylene dibromide that will measure by charging capacity drops into reactor, stirs and drops into diphenatril, Morpan BB down.Join alkali: according to the alkaline solution of charging capacity with sheet alkali preparation 60%.Stir cooling, temperature was no more than 80 ℃ in the control, finishes, and emits water coolant, stirs 1 hour, after temperature descends voluntarily in treating, begins to heat, and is warming up to 90 ℃, 90～95 ℃ of insulation reaction 5 hours.Insulation finishes, and is cooled to 50 ℃ with the chuck tap water, adds water and goes into reactor, continues to stir, and separates out crystallization, is cooled to below 10 ℃, leaves standstill more than 4 hours.Open the bottom valve blowing and in whizzer, get rid of material, wash to the water droplet that throws away with massive laundering and be neutral, continue to dry.Get rid of the material washing at every turn and all should wash most drying as far as possible.Take out that material places in the dish in the whizzer, tiling evenly puts that air seasoning place is dried or oven drying at low temperature, the bromotrifluoromethane diphenatril.
Embodiment 2: the quality that feeds intake proportioning such as following table:
| Name of material | Proportioning |
| Diphenatril | 1 |
| Ethylene dibromide | 2 |
| Morpan BB | 0.06 |
| Sheet alkali | 1.2 |
The concrete processing step of the preparation method of bromotrifluoromethane diphenatril of the present invention is:
Confirm reactor drying, cleaning, shut the reactor bottom valve, prepare to feed intake.The ethylene dibromide that will measure by charging capacity drops into reactor, stirs and drops into diphenatril, Morpan BB down.Join alkali: according to the alkaline solution of charging capacity with sheet alkali preparation 60%.Stir cooling, temperature was no more than 90 ℃ in the control, finishes, and emits water coolant, stirs 1.5 hours, after temperature descends voluntarily in treating, begins to heat, and is warming up to 90 ℃, 90～95 ℃ of insulation reaction 6 hours.Insulation finishes, and is cooled to 65 ℃ with the chuck tap water, adds water and goes into reactor, continues to stir, and separates out crystallization, is cooled to below 30 ℃, leaves standstill more than 4 hours.Open the bottom valve blowing and in whizzer, get rid of material, wash to the water droplet that throws away with massive laundering and be neutral, continue to dry.Get rid of the material washing at every turn and all should wash most drying as far as possible.Take out that material places in the dish in the whizzer, tiling evenly puts that air seasoning place is dried or oven drying at low temperature, the bromotrifluoromethane diphenatril.
Claims (5)
1. the preparation method of a bromotrifluoromethane diphenatril is characterized in that having following processing step: ethylene dibromide is dropped into reactor, stir and drop into diphenatril and Morpan BB down; To be that 60% alkaline solution slowly adds reactor with the concentration of sheet alkali preparation, temperature be no more than 90 ℃ in the control, finishes, and emits water coolant, stirs 45～90 minutes, after temperature descends voluntarily in treating, begins to heat, and is warming up to 90 ℃～98 ℃ insulation reaction 4～6 hours; Insulation finishes, and temperature is below 70 ℃ in being cooled to, and adds water and goes into reactor, continues to stir, separate out crystallization after, be cooled to below 30 ℃, leave standstill more than 4 hours, filter, wash with water to neutrality, dry or dry, get the bromotrifluoromethane diphenatril.
2. the preparation method of bromotrifluoromethane diphenatril according to claim 1 is characterized in that: after described alkaline solution adds reactor, emit water coolant after, the churning time that before heating up the raw material in the reactor is stirred is 60～70 minutes.
3. the preparation method of bromotrifluoromethane diphenatril according to claim 1 is characterized in that: after described insulation reaction finished, temperature was 40～55 ℃ in reactor was cooled to.
4. the preparation method of bromotrifluoromethane diphenatril according to claim 1 is characterized in that: after crystallization was separated out, temperature was 5～15 ℃ in the reactor cooling.
5. the preparation method of bromotrifluoromethane diphenatril according to claim 1 is characterized in that: the quality proportioning that feeds intake of described raw material is:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105664405A CN102030682A (en) | 2010-11-02 | 2010-12-01 | Preparation method of 4-bromo-2,2-diphenylbutyronitrile |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010527371.7 | 2010-11-02 | ||
| CN201010527371 | 2010-11-02 | ||
| CN2010105664405A CN102030682A (en) | 2010-11-02 | 2010-12-01 | Preparation method of 4-bromo-2,2-diphenylbutyronitrile |
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| Publication Number | Publication Date |
|---|---|
| CN102030682A true CN102030682A (en) | 2011-04-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105664405A Pending CN102030682A (en) | 2010-11-02 | 2010-12-01 | Preparation method of 4-bromo-2,2-diphenylbutyronitrile |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041583A (en) * | 1988-10-04 | 1990-04-25 | 美国辉瑞有限公司 | Muscarmic receptor antagonists |
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2010
- 2010-12-01 CN CN2010105664405A patent/CN102030682A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041583A (en) * | 1988-10-04 | 1990-04-25 | 美国辉瑞有限公司 | Muscarmic receptor antagonists |
Non-Patent Citations (2)
| Title |
|---|
| HOWARD P. NG,ET AL: "Discovery of Novel Non-Peptide CCR1 Receptor Antagonists", 《JOURNAL OF MEDICINAL CHEMISTRY》 * |
| 费楚华 等: "苯乙哌啶中间体的制备工艺改进", 《医药工业》 * |
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Application publication date: 20110427 |