Preparation method of dimethylaminocinnamaldehyde
A technology of p-dimethylaminocinnamaldehyde and p-chlorocinnamaldehyde, which is applied in the field of preparation of p-dimethylaminocinnamaldehyde, can solve the problems of high cost and high price, and achieve the effects of low cost, simple operation and high yield
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Embodiment 1
[0016] Before the addition, nitrogen purging was used to remove the oxygen in the reaction vessel, and then 100 g of aqueous sodium hydroxide solution with a mass fraction of 1% and 98 g of p-chlorobenzaldehyde were added, stirred and mixed thoroughly. Control the temperature at 20°C, add dropwise 55g of acetaldehyde aqueous solution with a mass fraction of 40% while stirring, dropwise for 45 minutes, control the temperature at 65°C after the dropwise addition, and react for 4 hours; after the reaction is completed, adjust to neutral with dilute hydrochloric acid , filtered to obtain crude product after cooling. Add 120g of ethanol to the crude product, then heat to 70°C, stir for half an hour, and put it into ice water to cool. After suction filtration, light yellow crystal p-chlorocinnamaldehyde with cinnamon bark odor was obtained, which was directly used in the next step reaction. The solid weighed 71 g after drying, and the yield was 86%.
[0017] In the reactor, adding...
Embodiment 2
[0019] Before the addition, nitrogen purging was used to remove the oxygen in the reaction vessel, and then 80 g of aqueous sodium hydroxide solution with a mass fraction of 1% and 84 g of p-chlorobenzaldehyde were added, stirred and mixed thoroughly. Control the temperature at 15°C, add dropwise 55g of acetaldehyde aqueous solution with a mass fraction of 40% while stirring, dropwise for 60 minutes, control the temperature at 63°C after the dropwise addition, and react for 3.5 hours; after the reaction is completed, adjust to neutral with dilute hydrochloric acid , filtered to obtain crude product after cooling. Add 100g of ethanol to the crude product, then heat to 70°C, stir for half an hour, then put it into ice water to cool. After suction filtration, light yellow crystal p-chlorocinnamaldehyde with cinnamon bark odor was obtained, which was directly used in the next step reaction. The solid weighed 70g after drying, and the yield was 85%.
[0020] In the reactor, addin...
Embodiment 3
[0022] Before the addition, nitrogen purging was used to remove the oxygen in the reaction vessel, and then 120 g of aqueous sodium hydroxide solution with a mass fraction of 1% and 100 g of p-chlorobenzaldehyde were added, stirred and mixed thoroughly. Control the temperature at 20°C, add dropwise 55g of acetaldehyde aqueous solution with a mass fraction of 40% while stirring, dropwise for 50 minutes, control the temperature at 62°C after the dropwise addition, and react for 5 hours; after the reaction is completed, use dilute hydrochloric acid to adjust to neutral , filtered to obtain crude product after cooling. Add 150g of ethanol to the crude product, then heat it to 70°C, stir for half an hour, and put it into ice water to cool. After suction filtration, light yellow crystal p-chlorocinnamaldehyde with cinnamon bark odor was obtained, which was directly used in the next step reaction. The solid weighed 73g after drying, and the yield was 88%.
[0023] In the reactor, a...
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