CN1958566A - Deodoration method in procedure for industrialized synthesizing chirality sulfenamide - Google Patents
Deodoration method in procedure for industrialized synthesizing chirality sulfenamide Download PDFInfo
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- CN1958566A CN1958566A CN 200610134284 CN200610134284A CN1958566A CN 1958566 A CN1958566 A CN 1958566A CN 200610134284 CN200610134284 CN 200610134284 CN 200610134284 A CN200610134284 A CN 200610134284A CN 1958566 A CN1958566 A CN 1958566A
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- sulfenamide
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- sulfolane
- hydrogen peroxide
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Abstract
This invention relates to a method for compound post-treatment, especially deodorization method for industrial synthesis of chiral sulfinyl amine. The invention connects an absorption container containing deodorant to the reaction kettle. The deodorant is sulfolane, H2O2, liquid paraffin, concentrated sulfuric acid, concentrated alkali or a mixture of sulfolane and H2O2. Sulfolane is stable in such systems as water, acid, alkali and oxygen, and has low volatility and toxicity. The absorption of sulfolane to acidic gases (including organic sulfides) is a physical dissolution one. The method has such advantages as easy operation, good absorption effect, shortened post-treatment time, and improved production efficiency, and is suitable for mass production.
Description
Technical field:
The present invention relates to the post-treating method of compound, particularly chiral sulfenamide synthetic post-treating method.
Background technology:
R (or S)-2-methyl-2-propyl group sulfinyl amine (tert-butanesulfinamide is called for short chirality tertiary butyl sulfinyl amine) is a very important chiral auxiliary(reagent) on medicine is synthetic.Synthesizing of chiral sulfenamide, though pass judgment on from the specialty chemical angle, this technology difficulty is little, but,, have the by product tert-butyl mercaptan to generate in synthesizing because the industrialization difficulty is big, understand the gas that discharges a small amount of low toxicity but unhappy smell is arranged, need equipment and operating process strict seal, the post-treatment condition harshness causes this compound can not scale operation.If can overcome the difficulty of this technology, synthetic at low cost in a large number this product is even will facilitate the new medicine of a large amount of new medicine intermediates to occur.
To this, Ellman
[1]Employing adds Mono Chloro Acetic Acid in reaction system, and in nitrogen environment, stirs under the room temperature and spend the night, tert-butyl mercaptan lithium and the good tert.-butylacetic acid lithium of Mono Chloro Acetic Acid lithium water generation reaction dissolubility that reaction is produced, and the taste removal principle is:
This method aftertreatment is a chemical action, and the treatment time is long, and cost is higher, has limited the industrialness synthetic and has extensively promoted.
Summary of the invention:
The objective of the invention is to overcome above-mentioned not enough problem, the deodorizing method in a kind of procedure for industrialized synthesizing chirality sulfenamide is provided, raw materials used rationally operation is simple, and effect is good.
The technical scheme that the present invention is adopted for achieving the above object is: the deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide, connect the absorption container that deodovization agent is housed behind reactor, deodovization agent is tetramethylene sulfone, hydrogen peroxide, whiteruss, the vitriol oil, concentrated base or tetramethylene sulfone and hydrogen peroxide mixed solution etc.
Described deodovization agent is that tetramethylene sulfone and hydrogen peroxide are loaded on two independent absorptions in the container.
Described deodovization agent be tetramethylene sulfone and hydrogen peroxide by 1: the mixing solutions of 1-3 volume ratio.
Described hydrogen peroxide concentration is 25-30%.
Deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide of the present invention, select for use absorption agents such as tetramethylene sulfone, hydrogen peroxide to absorb, particularly tetramethylene sulfone is all stable to water, acid, alkali and oxygen etc., volatility is little, nontoxic, be the physical dissolution effect to the absorption of sour gas (including organic sulfur compound).Simple to operation, and assimilation effect is good, shortens the post-reaction treatment time, improves industrial production efficiency, is suitable for the large-scale production of industrialization, enlarges the range of application of sulfinyl amine.
Embodiment:
The present invention is described in further detail below in conjunction with specific embodiment, but be not limited to following
Embodiment.
Embodiment 1
Deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide, whole reaction system is airtight, leak without any peculiar smell, when the question response thing becomes solid, stop to stir, after main reaction finishes, in still, add quencher (ethanol, water, ammonium chloride saturated solution or buck etc.) cancellation, when beginning ammonia excretion gas in the reactor, airway is connected in turn two independent containers that absorb of the hydrogen peroxide that tetramethylene sulfone and concentration 25% are housed, system band vacuum, in the exhaust process of ammonia, the tert-butyl mercaptan of carrying secretly is through absorbing container, and stink is absorbed, the ammonia that discharges again is discharged in the water pump, and smell is all removed.
Embodiment 2
Deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide, whole reaction system is airtight, leak without any peculiar smell, when the question response thing becomes solid, stop to stir, after main reaction finishes, in still, add the saturated ammonium chloride solution cancellation,, be connected to airway in turn hydrogen peroxide that concentration 25% is housed and two of tetramethylene sulfone absorb containers separately when in the reactor during beginning ammonia excretion gas, system band vacuum, in the exhaust process of ammonia, the tert-butyl mercaptan of carrying secretly is through absorbing container, and stink is absorbed, the ammonia that discharges again is discharged in the water pump, and smell is all removed.
Embodiment 3
Deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide, after main reaction finishes, in reactor, add the ethanol cancellation, when beginning ammonia excretion gas in the reactor, airway is communicated with the absorption container, the tetramethylene sulfone of 1: 1 ratio and the mixing solutions of 30% hydrogen peroxide are housed in the container, system band vacuum, in the exhaust process of ammonia, the tert-butyl mercaptan of carrying secretly is through absorbing container, stink is thoroughly sponged, the odorlessness when ammonia that discharges again is discharged in the water pump.
Embodiment 4
Deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide, after main reaction finishes, in reactor, add shrend and go out, when beginning ammonia excretion gas in the reactor, airway is communicated with the absorption container, the tetramethylene sulfone of 1: 2 ratio and the mixing solutions of 28% hydrogen peroxide are housed in the container, system band vacuum, in the exhaust process of ammonia, the tert-butyl mercaptan of carrying secretly is through absorbing container, stink is thoroughly sponged, the odorlessness when ammonia that discharges again is discharged in the water pump.
Claims (4)
1, the deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide is characterized in that: connect the absorption container that deodovization agent is housed behind reactor, deodovization agent is tetramethylene sulfone, hydrogen peroxide or tetramethylene sulfone and hydrogen peroxide mixed solution.
2, the deodorizing method in the procedure for industrialized synthesizing chirality sulfenamide according to claim 1 is characterized in that: deodovization agent is that tetramethylene sulfone and hydrogen peroxide are loaded on two independent absorptions in the container.
Deodorizing method in 3 procedure for industrialized synthesizing chirality sulfenamide according to claim 1 is characterized in that: deodovization agent be tetramethylene sulfone and hydrogen peroxide by 1: the mixing solutions of 1-3 volume ratio.
4 according to the deodorizing method in the arbitrary described procedure for industrialized synthesizing chirality sulfenamide of claim 1-3, and it is characterized in that: hydrogen peroxide concentration is 25-30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134284 CN1958566A (en) | 2006-11-13 | 2006-11-13 | Deodoration method in procedure for industrialized synthesizing chirality sulfenamide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610134284 CN1958566A (en) | 2006-11-13 | 2006-11-13 | Deodoration method in procedure for industrialized synthesizing chirality sulfenamide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1958566A true CN1958566A (en) | 2007-05-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610134284 Pending CN1958566A (en) | 2006-11-13 | 2006-11-13 | Deodoration method in procedure for industrialized synthesizing chirality sulfenamide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1958566A (en) |
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2006
- 2006-11-13 CN CN 200610134284 patent/CN1958566A/en active Pending
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