Diazomethane on-line deriving method

Abstract

The invention relates to a diazomethane on-line deriving method, which comprises the following steps of: (1) a step of generating diazomethane; and (2) a step of deriving the diazomethane. The method can be realized under the action of N2. The method also comprises a tail gas absorption step after the step of deriving the diazomethane, wherein absorbent used in the tail gas absorption step for absorbing excessive diazomethane can be aether. The method also comprises a N2 flow rate control step before the step of generating the diazomethane and also comprises a diazomethane gas distribution step between (1) the step of generating the diazomethane and (2) the step of deriving the diazomethane. The method can be carried out in sealed environment. The diazomethane on-line deriving method can also comprise a step of exhausting the exhaust gas generated in the reaction from the sealed environment. The method organically integrates the preparation and the derivation of the diazomethane and has the characteristics of safety and high efficiency.

Description

technical field [0001] The invention relates to an on-line derivation method of diazomethane. Background technique [0002] At present, most of the data at home and abroad use the method of firstly preparing the diazomethane solution, and then using the prepared diazomethane solution for derivation. Its preparation process and principle are: [0003] Place the double-necked distillation flask containing the mixture of potassium hydroxide, ethanol and anhydrous ether in a water bath on a heating plate of a magnetic stirrer, and the water temperature is 70°C. Connect the dropping funnel and high-efficiency condenser, and connect the receiving bottle in series after condensing the pipeline. Put anhydrous ether in the absorption flask. Add N-methyl-nitroso-p-toluenesulfonamide anhydrous ether solution dropwise under stirring, and the dropping time is controlled over 20 minutes. Stop distillation when the solution in the distilling bottle is light yellow. The liquid in the r...

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Problems solved by technology

[0004] The preparation method of diazomethane in the above prior art is relatively complicated, and there is no continuity between preparation and derivation, so many people try to use the simple process of "continuous bubbling" to realize the derivation operation of organic acid compounds. Such as EPA 8151A, but in view of the explosiveness and carcinogenicity of diazomethane itself, many people talk about it. In addition, the safety of the bubbling method itself cannot be guaranteed, and the efficiency, efficiency and stability of the method itself cannot be guaranteed. , so this type of method does not solve the problem of how to effectively and safely prepare diazomethane and its integration with diazomethane derivatives in the prior art

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