High-yield ethyl chrysanthemate preparation method
A high-yield technology of ethyl chrysanthemum acid, applied in the field of chemical technology, can solve the problem of low chemical yield, and achieve the effects of reducing poisoning and excellent environmental protection performance
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[0037] Example 1
[0038] A method for preparing ethyl chrysanthenate with high yield, comprising the following steps:
[0039] (1) diazotization: put in 600 parts of water, 490 parts of glycine ethyl acetate and 35 parts of glacial acetic acid in the diazotization kettle, stir to dissolve the solid, and adopt glacial acetic acid to keep the pH value of the diazotization reaction at 3.5~ Between 4.5, then put 800 parts of dimethyl carbonate into the diazotization kettle as a solvent, open the freezing, make the temperature of the material in the diazotization kettle drop to 20~25 ℃, and then drop the sodium nitrite aqueous solution in the diazotization kettle. , the dropwise addition time of sodium nitrite is controlled at 4~5h, after the dropwise addition, the temperature is kept for 60min, after the reaction is completed, static layering is performed, and the lower water layer is discharged to the waste liquid collection tank, that is, the diazo liquid is obtained;
[0040]...
Example Embodiment
[0051] Example 2
[0052] The difference between embodiment 2 and embodiment 1 is:
[0053] (1) diazotization: put in 500 parts of water, 480 parts of glycine ethyl acetate and 36 parts of glacial acetic acid in the diazotization kettle, stir to dissolve the solid, and adopt glacial acetic acid to keep the pH value of the diazotization reaction at 3.5~ Between 4.5, then put 800 parts of dimethyl carbonate into the diazotization kettle as a solvent, open the freezing, make the temperature of the material in the diazotization kettle drop to 20~25 ℃, and then drop the sodium nitrite aqueous solution in the diazotization kettle. , the dropwise addition time of sodium nitrite is controlled at 4~5h, after the dropwise addition, the temperature is kept for 45min, after the reaction is completed, static layering is performed, and the lower water layer is discharged to the waste liquid collection tank, that is, the diazo liquid is obtained;
[0054] (2) Cyclization: put 1,100 parts of...
Example Embodiment
[0055] Example 3
[0056] The difference between Example 3 and Example 1 is:
[0057] (1) diazotization: put 700 parts of water, 470 parts of glycine ethyl acetate and 37 parts of glacial acetic acid in the diazotization kettle, stir to dissolve the solid, and adopt glacial acetic acid to keep the pH value of the diazotization reaction at 3.5~ Between 4.5, then put 800 parts of dimethyl carbonate into the diazotization kettle as a solvent, open the freezing, make the temperature of the material in the diazotization kettle drop to 20~25 ℃, and then drop the sodium nitrite aqueous solution in the diazotization kettle. , the dropwise addition time of sodium nitrite is controlled at 4~5h, after the dropwise addition, the temperature is kept for 60min, after the reaction is completed, static layering is performed, and the lower water layer is discharged to the waste liquid collection tank, that is, the diazo liquid is obtained;
[0058] (2) Cyclization: put 1100 parts of 2,5-dimet...
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