Deodoration method in procedure for industrialized synthesizing chirality sulfenamide

A sulfenamide and chiral technology, which is applied in the post-treatment field of chiral sulfenamide synthesis, can solve the problems of restricting the widespread promotion of industrial synthesis, high cost, and long processing time, and achieve shortened processing time and low volatility , good absorption effect

Inactive Publication Date: 2007-05-09
DALIAN NETCHEM CHIRAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The post-treatment of this method is chemical action, the processing time is long, and the cost is high, which limits the wide promotion of industrial synthesis

Method used

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  • Deodoration method in procedure for industrialized synthesizing chirality sulfenamide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The deodorization method in the process of industrial synthesis of chiral sulfinamides. The whole reaction system is airtight without any peculiar smell leakage. When the reactant becomes solid, stop stirring. After the main reaction is finished, add a quencher (ethanol, water, ammonium chloride saturated solution or alkaline water, etc.), when the ammonia gas in the reaction kettle starts to be exhausted, connect the air guide tube to two separate absorption containers containing sulfolane and hydrogen peroxide with a concentration of 25% in sequence, and the system is vacuumed , During the exhaust process of ammonia gas, the entrained tert-butyl mercaptan passes through the absorption container, and the odor is absorbed, and then the discharged ammonia gas is discharged into the water pump, and the odor is completely removed.

Embodiment 2

[0017] The deodorization method in the process of industrial synthesis of chiral sulfinamides. The entire reaction system is airtight without any odor leakage. When the reactants become solid, stop stirring. After the main reaction is completed, add saturated ammonium chloride solution to the kettle to quench When the ammonia gas is exhausted in the reaction kettle, connect the gas guide tube to two separate absorption containers containing 25% hydrogen peroxide and sulfolane in sequence, and the system is vacuumed. During the exhausting process of ammonia gas, the entrained tertiary Butyl mercaptan passes through the absorption container, the odor is absorbed, and then the discharged ammonia gas is discharged into the water pump, and the odor is completely removed.

Embodiment 3

[0019] The deodorization method in the process of industrial synthesis of chiral sulfinamides. After the main reaction is completed, ethanol is added to the reaction kettle to quench. When the ammonia gas is discharged from the reaction kettle, the air guide pipe is connected to the absorption container. The container is equipped with 1 : A mixed solution of sulfolane and 30% hydrogen peroxide in a ratio of 1. The system is vacuumed. During the exhausting process of ammonia gas, the entrained tert-butyl mercaptan passes through the absorption container, the odor is completely absorbed, and then the ammonia gas is discharged Odorless when discharged into the pump.

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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: [0001] The invention relates to a post-treatment method for compounds, in particular to a post-treatment method for the synthesis of chiral sulfinamides. Background technique: [0002] R (or S)-2-methyl-2-propyl sulfinamide (tert-butanesulfinamide, referred to as chiral tert-butyl sulfinamide) is a very important chiral auxiliary in pharmaceutical synthesis. The synthesis of chiral sulfinamides, although judged from the perspective of chemical expertise, the process is not difficult, but due to the difficulty of industrialization, the by-product tert-butyl mercaptan is generated during the synthesis, which will release a small amount of low toxicity but has an unpleasant smell The gas needs to be strictly sealed in equipment and operation process, and the post-treatment conditions are harsh, so the compound cannot be produced on a large scale. If the difficulty of the process can be overcome, the product can be synthesized in large quantities at low cost, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/44C07C313/06
Inventor 吴星娥陈有刚王维新张乙郑烈
Owner DALIAN NETCHEM CHIRAL TECH
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