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Method for determining productivity of diazomethane and method for preparing diazomethane

A diazomethane and yield technology, applied in the preparation of test samples, material separation, instruments, etc., can solve the problem of reducing the yield of diazomethane and its conversion products, low yield of diazomethane, and reducing the yield of diazomethane Problems such as rate accuracy, to achieve the effect of safety inspection of diazomethane yield

Inactive Publication Date: 2014-03-12
BAYER TECH & ENG SHANGHAI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when this method utilizes micro-reaction technology to eliminate potential safety hazards, due to the generation of side reactions, the yield of diazomethane and its conversion products is reduced, and the accuracy of checking the yield of diazomethane is reduced.
The yield of diazomethane detected by this method disclosed in this document is generally lower than 50%, and the highest yield is only 75%

Method used

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  • Method for determining productivity of diazomethane and method for preparing diazomethane

Examples

Experimental program
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Effect test

preparation example Construction

[0029] The method for preparing diazomethane disclosed by the present invention comprises the steps of:

[0030] The dimethyl sulfoxide solution of the N-nitroso compound or the mixed solution of dimethyl sulfoxide and ether and the methanol solution of the strong base are mixed and reacted in the first micro-reaction device to obtain the first mixture including diazomethane . The first micro-reaction device preferably consists of a micro-mixer and a capillary micro-reactor. The time of the mixing reaction in the micro-mixer is extremely short, most of the reactions are carried out in the capillary microreactor, the total mixing reaction time is 10s~50s, and the mixing reaction is carried out in the first micro-reaction device The temperature ranges from 15°C to 45°C;

[0031] A sample of the first reaction mixture comprising diazomethane is mixed with the methanol solution of alkyl acetic acid or benzoic acid in the second micro-reaction device to obtain the second mixture ...

Embodiment 1

[0051] (1) At first, the dimethyl sulfoxide solution of the dimethylnitrosobenzene sulfonamide of 0.3mol / L is mixed with the methanol solution of 0.45mol / L potassium hydroxide in a micro mixer, and then the mixed The reaction mixture is passed into a capillary microreactor with an internal diameter of 1 mm to continue the reaction, and the reaction generates a diazomethane reaction mixture. The micromixer and the capillary microreactor are placed in a water bath, the reaction temperature is 20 ° C, and the reaction time is 39.2 s, the volumetric flow rate is 24ml / min.

[0052] (II) Then, the above-mentioned diazomethane reaction mixture is mixed with the methanol solution of 1.2mol / L isobutyric acid in another micromixer, and then the mixed reaction mixture is passed into a capillary microreactor with an internal diameter of 2mm Continue the reaction in the middle of the reaction to generate a reaction mixture of methyl isobutyrate. The micro-mixer and capillary micro-reactor ...

Embodiment 2～5

[0055] Compared with Example 1, except that the variables shown in the following table changed, Examples 2-5 adopted basically the same experimental device and basically the same experimental steps to achieve a high yield similar to that of Example 1.

[0056]

[0057] Compared with the prior art, the above examples disclose a relatively accurate method for measuring the yield of diazomethane within a certain range of data and a method for preparing diazomethane in a safe, continuous and high-yield manner, which is an important contribution to the diazomethane industry. The expansion of production on the Internet provides a feasible operation plan.

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Abstract

The invention relates to a method for determining productivity of diazomethane and a method for preparing the diazomethane. The method for determining productivity of diazomethane comprises the steps that mixing a product sample of the diazomethane with methanol solution of alkyl acetic acid or benzoic acid in a micro reacting device to react so as to obtain mixture containing alkyl methyl ester or benzoic acid methyl ester, and then detecting yield of the alkyl methyl ester or the benzoic acid methyl ester in the mixture to calculate the productivity of the diazomethane. The methods can accurately determine the productivity of the diazomethane and produce and prepare the diazomethane in industrialized, continuous, high-efficiency and safe mode.

Description

technical field [0001] The invention relates to a method for determining the yield of diazomethane and a method for preparing diazomethane. Background technique [0002] Diazomethane is an important intermediate in organic synthesis and has very important applications in the pharmaceutical field. Due to its strong reactivity, diazomethane can be used as a methylating reagent to react with compounds with active hydrogen atoms such as carboxylic acids and phenols to generate corresponding methyl esters or methyl ethers, with the only accompanying by-product nitrogen . However, since diazomethane is an unstable yellow gas at room temperature, it is highly carcinogenic, highly toxic, and flammable and explosive, which increases operational difficulty and safety hazards in the preparation, storage and use processes. [0003] US5817778A discloses a batch reaction method for preparing diazomethane and checking the yield of diazomethane. The method is to slowly drop dimethylnitro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N21/33G01N1/38C07C245/16
Inventor 何宽段学志周兴贵钱刚
Owner BAYER TECH & ENG SHANGHAI
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