Diazomethane on-line deriving method

A technology of diazomethane and p-toluenesulfonamide, applied in chemical instruments and methods, formation/introduction of ether group/acetal group/ketal group, formation/introduction of carboxylate group, etc., can solve method efficiency Efficiency and stability cannot be guaranteed, preparation and derivation have no continuity, and the safety of the bubbling method cannot be guaranteed, etc., to achieve the effect of improving the operability and reproducibility of derivation, enhancing safety and operability, and improving reproducibility

Inactive Publication Date: 2010-05-12
INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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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 diazo...

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  • Diazomethane on-line deriving method
  • Diazomethane on-line deriving method
  • Diazomethane on-line deriving method

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Embodiment Construction

[0048] See attached figure 1 , figure 2 , a diazomethane online derivation method is characterized in that it comprises the following steps: (1), a diazomethane generation step; (2), a diazomethane derivation step.

[0049] (1) The diazomethane generation step includes: adding the mixed solution including potassium hydroxide, alcohol and ether mixture, etc. into the N methyl-nitroso-p-toluenesulfonamide solid at normal temperature to prepare diazomethane gas . (2) The diazomethane derivation step includes: reacting diazomethane gas with organic matter at room temperature to prepare corresponding esters. The diazomethane online derivation method is realized under the impetus of N2. After the (2) diazomethane derivatization step, a tail gas absorption step is also included. The absorbent used in the tail gas absorption step to absorb excess diazomethane is diethyl ether. (1) The N2 flow control step is also included before the diazomethane generating step. A diazomethane ...

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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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Application Information

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IPC IPC(8): C07B41/12C07B41/04C07C69/712C07C67/00C07C205/37C07C201/12C07C43/225C07C41/01
Inventor 桂建业张莉张永涛左海英
Owner INST OF HYDROGEOLOGY & ENVIRONMENTAL GEOLOGY CHINESE ACAD OF GEOLOGICAL SCI
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