A kind of 3-n, the preparation method of n-dimethylamino ethyl acrylate
A technology of ethyl dimethylaminoacrylate and ethyl formoacetate sodium salt, which is applied in the field of 3-N, can solve the problems of long reaction time, high cost, and many wastes, and achieve the goal of reducing operation difficulty and danger, and reducing operation risk Effect
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Embodiment 1
[0019] 1), the preparation of ethyl formoacetate sodium salt
[0020] Add 68g of sodium ethoxide, 160g of toluene, 140g of ethyl acetate and 0.3g of piperidine into the autoclave, start stirring, fill the autoclave with carbon monoxide to increase the pressure, and heat it at the same time, and control the temperature of the autoclave to 65°C-70°C , raise the pressure of carbon monoxide in the reactor to 12bar, and react for 4hrs. After the reaction, slowly release the pressure to normal pressure, cool the reaction solution to 0°C, grow crystals for 1hr, filter with suction, stir and wash with 100ml of absolute ethanol three times 131.8 g of ethyl formoacetate sodium salt was obtained, and the yield was 95.5% (compared to sodium ethoxide);
[0021] 2) Preparation of 3-N, N-ethyl dimethylaminoacrylate
[0022] Add the ethyl formyl acetate sodium salt obtained in step 1) to 280 g of a 35% dimethylamine hydrochloride aqueous solution, during which the temperature is controlled a...
Embodiment 2
[0024] 1), the preparation of ethyl formoacetate sodium salt
[0025] Add 68g of sodium ethoxide, 160g of toluene, 140g of ethyl acetate and 1.3g of piperidine into the autoclave, start stirring, fill the autoclave with carbon monoxide to raise the pressure, and heat it at the same time, and control the temperature of the autoclave to 55°C-60°C ℃, and the pressure of carbon monoxide in the reactor was raised to 10 bar, and reacted for 4 hrs. After the reaction was completed, the pressure was slowly released to normal pressure, the temperature of the reaction solution was lowered to 0° C., and the crystal was grown for 1 hr. Suction filtration, stirring and washing with ethanol three times to obtain 128.1 g of ethyl formoacetate sodium salt with a yield of 92.8% (compared to sodium ethoxide);
[0026] 2) Preparation of 3-N, N-ethyl dimethylaminoacrylate
[0027] Add the ethyl formyl acetate sodium salt obtained in step 1) to 275 g of a 35% aqueous solution of dimethylamine hy...
Embodiment 3
[0028] Embodiment 3 (comparative example)
[0029] Same as step 1) in Example 1, except that piperidine was not used as a catalyst to obtain 39.6 g of ethyl formoacetate sodium salt with a yield of 28.7%, and a large amount of ethyl acetoacetate by-product was generated by gas phase detection.
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