Glycerinum ternary aldehyde and synthesis method thereof
A technology of glycerol trialdehyde and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of complex and difficult reaction conditions, single source of raw materials, and complicated operation steps, and achieves the synthesis route. Simple, high industrial value, easy to operate effect
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Embodiment 1
[0031] This embodiment relates to a novel structure of glycerol tri-aldehyde and its synthesis method, such as figure 1 As shown, among them, equiv means equivalent. Concrete synthetic steps are as follows:
[0032] (1) Preparation and purification of trihydric glycerol
[0033] In a three-neck round bottom flask, add solvent 1,2-dichloromethane (200mL) and glyceryl trioleate (20.05g, 22.64mmol), stir, lower the temperature of the system to -78°C, and introduce O 3 Stop feeding O until the mixture turns light blue (about 17 minutes, q≥5L / min). 3 , pass into O 2 / N 2 to remove excess O3 ( 10 minutes, q≥5L / min); add tetrahydrofuran (80mL), sodium borohydride (20.56g, 543.46mmol, 16equiv), react at -78°C for 30 minutes, heat up at room temperature for 10 minutes, and then ice-bath for 90 minutes , and finally stirred at room temperature for 1-12 hours.
[0034] After the reaction, use a sand core funnel to filter off excess sodium borohydride, and remove CH by rotary evapo...
Embodiment 2
[0041] This embodiment relates to novel ternary aldehydes and their synthesis, separation and purification methods, such as figure 2 As shown, among them, equiv means equivalent. Concrete synthesis, separation and purification steps are as follows:
[0042] (1) Preparation and purification of trihydric glycerol
[0043] In a three-neck round bottom flask, add solvent 1,2-dichloromethane (200mL) and glyceryl trioleate (20.81g, 23.50mmol), stir, lower the temperature of the system to -78°C, and introduce O 3 Stop feeding O until the mixture turns light blue (about 17 minutes, q≥5L / min). 3 , pass into O 2 / N 2 to remove excess O 3 (10 minutes, q≥5L / min); add isopropanol (80mL), sodium borohydride (21.34g, 564.06mmol, 16equiv), react at -78°C for 30 minutes, warm up at room temperature for 10 minutes, then ice Bath for 90 minutes, and finally stir the reaction at room temperature for 1-12 hours.
[0044] After the reaction, use a sand core funnel to filter off excess sodiu...
Embodiment 3
[0051] This example uses rapeseed oil as a raw material and relates to a novel glycerol trialdehyde and its synthesis method, wherein equiv represents equivalent. Concrete synthetic steps are as follows:
[0052] (1) Preparation and purification of trihydric glycerol
[0053] In a three-neck round bottom flask, add the solvent 1,2-dichloromethane (100mL) and rapeseed oil (10.03g, 11.33mmol, calculated as triolein), stir, and lower the temperature of the system to -78°C , feed 03 until the mixture turns light blue (about 15 minutes, q≥5L / min), stop feeding O 3 , pass into O 2 / N 2 to remove excess O 3 (10 minutes, q≥5L / min); add tetrahydrofuran (40mL), sodium borohydride (10.29g, 271.92mmol, 16equiv), react at -78°C for 30 minutes, heat up at room temperature for 10 minutes, then ice-bath for 90 minutes, and finally stirred at room temperature for 1-12 hours.
[0054] After the reaction, use a sand core funnel to filter off excess sodium borohydride, and remove CH by rota...
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