A new method for synthesizing dialdehyde compounds
A compound, glutaraldehyde technology, applied in the field of synthesis of dialdehyde compounds, can solve problems such as unsuitable for industrial production, expensive raw materials, unsafe factors, etc., achieve short reaction completion time, high product purity, and high reactivity Effect
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Embodiment 1
[0057] Embodiment 1, the synthesis of succinic dialdehyde
[0058] The reaction formula is as follows:
[0059]
[0060] Add magnesium strips (0.11mol) to a 250mL flask, add 10mL tetrahydrofuran to cover the surface of the magnesium strips, add iodine crystals, dissolve acetal A (0.1mol) in 40mL tetrahydrofuran, and drop 1 / 10 of it into the magnesium strips , to initiate the reaction, and the rest of the liquid was added dropwise at 40-45°C, and the drop was completed in about 2 hours, and the stirring was continued for 0.5 hour, and the residual magnesium strips were filtered off to obtain the Grignard reagent.
[0061] Drop the Grignard solution into 10 mL of tetrahydrofuran mixed solution of acetal A (0.1 mol), reflux for 2 hours after dropping, add 10wt% acetic acid aqueous solution, continue stirring for 1 hour, add dichloromethane and water for extraction, combine the organic phases, Drying and concentrating gave succinic dialdehyde (boiling point 56.0-56.6°C) with a...
Embodiment 2
[0062] Embodiment 2, the synthesis of succinic dialdehyde
[0063] The reaction formula is as follows:
[0064]
[0065] Add magnesium strips (0.11mol) to a 250mL flask, add 10mL tetrahydrofuran to cover the surface of the magnesium strips, add iodine crystals, dissolve acetal B (0.1mol) in 40mL tetrahydrofuran, and drop 1 / 10 of it into the magnesium strips , to initiate the reaction, and the rest of the liquid is added dropwise at 40-45°C, and the drop is completed in about 2 hours, and the stirring is continued for 0.5 hour, and the Grignard reagent is obtained by the reaction.
[0066] Drop the Grignard solution into 10 mL of tetrahydrofuran mixed solution of acetal A (0.1 mol), reflux for 2 hours after dropping, add 10wt% acetic acid aqueous solution, continue stirring for 1 hour, add dichloromethane and water for extraction, combine the organic phases, Drying and concentrating gave succinic dialdehyde (boiling point 55.7-56.5°C) with a yield of 82% and a purity of ≥98...
Embodiment 3
[0067] Embodiment 3, the synthesis of succinic dialdehyde
[0068] The reaction formula is as follows:
[0069]
[0070] Add magnesium strips (0.11mol) to a 250mL flask, add 10mL of anhydrous ether to cover the surface of the magnesium strips, add iodine crystals, dissolve acetal C (0.1mol) in 40mL of anhydrous ether, and drop 1 / 10 of it Put it into the magnesium strips to initiate the reaction, then add the rest of the liquid dropwise at 25-30°C, and the dripping is completed in about 2 hours, and continue to stir for 0.5 hours, and filter off the residual magnesium strips to obtain the Grignard reagent.
[0071] Drop the Grignard solution into 10 mL of anhydrous ether mixture of acetal D (0.1 mol), reflux for 2 hours after dropping, add 10wt% acetic acid aqueous solution, continue stirring for 1 hour, add dichloromethane and water for extraction, combine organic phase, dried and concentrated to obtain succinic dialdehyde (boiling point 56.2-57.1 °C), with a yield of 82% ...
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