Synthesis of potassium acetylsulfanilate

A technology of acesulfame potassium and dichloroethane, applied in the field of synthesis and preparation of acesulfame potassium, can solve the problems of difficult removal, long reduction time, explosion, etc., and achieves short reaction time, easy three-waste treatment, and technological method easy effect

Inactive Publication Date: 2002-02-20
张元宾 +1
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Problems solved by technology

[0010] In this patent, deficiency one: the first (2) step uses NaN 3 For the generated azide, when distilling the solvent, the temperature should not exceed 25°C, otherwise it will easily cause an explosion. If the temperature does not exceed 25°C, the residual solvent is not easy to remove, which will affect the next reaction and yield
Weakness two: the first (3) step with NaBH 4 To reduce azide, the reducing agent used NaBH 4 Insoluble in tetrahydrofuran, only its suspension can be used, the reduction time is very long, the effect is not ideal, and the yield fluctuates.

Method used

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Embodiment Construction

[0021] Further describe the present invention in detail with embodiment below:

[0022] The synthetic preparation method of acesulfame potassium is characterized in that:

[0023] (1) Preparation of substituted phenoxysulfonyl chlorides: substituted phenoxysulfonyl chlorides are prepared by reacting substituted sodium phenolate or substituted phenols with sulfonyl chlorides, the reaction temperature is -10°C to 20°C, and halogenated with alkyl or alkoxy groups Ammonium is used as a catalyst, and the reaction is carried out in a solvent of alkyl aromatic hydrocarbon or halogenated alkanes;

[0024] (2) Preparation of substituted phenoxysulfonamide: In the reaction tower, dissolve the substituted phenoxysulfonyl chloride in a solvent of halogenated alkanes, cool to -5°C ~ +30°C, and control the pressure at 2 ~ 10Mpa, Under the action of a catalyst, feed liquid ammonia or ammonia gas to react;

[0025] (3) Preparation of acetoacetamido-N-sulfonyl-substituted phenoxy group: reac...

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Abstract

The present invention relates to the preparation of acetyl potassium sulfanilate; preparation of substituted phenoxy sulfamide; preparation of acetyl acetoamino-N-sulfuryl-substituted phenoxyl; preparation of acetyl potassium sulfanilate. The present invention is simple in technology, relatively short reaction time, easy treatment of wastes.

Description

(1) Technical field [0001] The invention relates to a method for preparing chemical substances, in particular to a method for synthesizing and preparing acesulfame potassium. (2) Background technology [0002] The chemical synthesis method of acesulfame potassium has the following several at present: [0003] (1) With fluorine or chlorosulfonyl isocyanate (FSO 2 NCO or ClSO 2 NCO) reacts with isobutyl acetoacetate. In this method, the intermediate chlorosulfonyl isocyanate needs to be prepared with highly toxic NaCN. Because NaCN is a highly toxic drug and is prone to personal death, it is not suitable for industrial production. In addition, this reaction is carried out at low temperature, which consumes a lot of energy and increases the cost of the product. Therefore, this method is not suitable for industrial production. [0004] (2) Reaction of acetoacetamide with fluorosulfonyl. [0005] (3) Diketene reacts with aminofluorosulfonyl. [0006] In (2), (3) method, SO ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D291/06
CPCC07D291/06
Inventor 田年寿刘海明
Owner 张元宾
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