A method for stably and efficiently preparing n-acrylamide compounds
A technology for acrylamide and compounds, which is applied in the field of stable and efficient preparation of N-acrylamide compounds, can solve the problems of product loss, easy polymerization reaction, time-consuming and complicated water removal process, etc.
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Embodiment 1
[0040] First, 88.4 g of anhydrous potassium carbonate was dissolved in 320 mL of deionized water, and cooled to room temperature. Then add 60g of glycinamide hydrochloride and stir to dissolve, then add 64mL of acetonitrile.
[0041] figure 2 (a) mixed solvent system in the prior art, figure 2 (b) is the mixed solvent system of the present invention. It can be seen that in the reaction solvent system of the prior art, acryloyl chloride is dissolved in an organic solvent, and glycinamide hydrochloride is dissolved in water, so acryloyl chloride and glycinamide hydrochloride are only The reaction occurs at the interface of organic solvent and water. However, in the reaction solvent system provided by the present invention, acryloyl chloride and glycinamide hydrochloride can not only react at the interface between the organic solvent and water, but also because the organic solvent used in the present invention can disperse acryloyl chloride into water, making the reaction pro...
Embodiment 2
[0047] First, 72.96 g of anhydrous sodium carbonate was dissolved in 320 mL of deionized water, and cooled to room temperature. Then add 60g of glycinamide hydrochloride and stir to dissolve, then add 64mL of acetone. Then the reaction solution was cooled to 10°C, and acryloyl chloride diluted with acetonitrile (44mL of acryloyl chloride diluted with 176mL of acetone) was slowly added dropwise for about 6 hours, during which the temperature of the reaction solution was kept at 5-15°C. The reaction was then continued at room temperature 20-30° C. for 1 h. After the reaction was completed, the reaction solution was spin-dried, and then 200 mL of methanol and 800 mL of ethanol were added successively to extract the product and precipitate salts. After filtering, the filtrate was spin-dried. Then, a mixed solvent of 10 mL of methanol, 200 mL of ethyl acetate and 200 mL of n-hexane was added to wash away impurities, filtered, and the resulting solid was dried at 55° C. for 12 h to...
Embodiment 3
[0049] Compared with the preparation of N-acryloyl glycinamide using a mixed solvent of ether and water in the prior art, the present invention has good stability, and also uses an organic solvent stored for 2 months. In the preparation method of the mixed solvent of ether and water, polymerization occurred 4 times in 5 times, and a hydrogel with unknown monomer concentration was formed before the monomer was obtained, as shown in the attached figure 1 Shown is a physical picture of gel formation due to polymerization during the preparation of N-acryloyl glycinamide using ether as an organic solvent in the prior art. However, no polymerization occurred in the mixed solvent system proposed by the present invention.
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