Carboxylic ester structure containing diene monomer and polyester thereof, and sulfur-containing polyester
A sulfur-containing polyester and carboxylate technology, which is applied in the field of carboxylate-containing diene monomers and their polyesters and sulfur-containing polyesters, can solve the problems of non-renewable, limited fossil resources, and environmental pollution of fossil resources. , to achieve the effect of easy production, simple synthesis process and reduced dependence
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[0079] Example 1
[0080] The allylation reaction of p-hydroxybenzaldehyde, the reaction equation is as follows:
[0081]
[0082] Experimental steps:
[0083] Add p-hydroxybenzaldehyde (100 mmol) to the flask and dissolve it in 50 ml of absolute ethanol. Add anhydrous potassium carbonate (150 mmol) and stir at room temperature for 30 min. Add bromopropene (120 mmol) dropwise under a nitrogen atmosphere. ), the molar ratio of p-hydroxybenzaldehyde to bromopropylene to anhydrous potassium carbonate is 1:1.2:1.5. After the addition, the temperature is gradually increased to 80°C, condensed and refluxed, reacted for 72h, filtered, and the solvent is removed under reduced pressure distillation , Diluted with a small amount of water, extracted with ethyl acetate and saturated brine. Combine the organic phases, add anhydrous sodium sulfate, let stand overnight, collect on silica gel dry method, use a mixed solvent of petroleum ether / ethyl acetate (volume ratio 6:1) as the eluent for chro...
Example Embodiment
[0084] Example 2
[0085] The allylation reaction of vanillin monomer, the reaction equation is as follows:
[0086]
[0087] Experimental steps:
[0088] Add vanillin (150 mmol) to the flask and dissolve it in 80 ml of absolute ethanol, add anhydrous potassium carbonate (750 mmol) and stir at room temperature for 30 min, add bromopropene (180 mmol) dropwise under a nitrogen atmosphere, The molar ratio of vanillin to bromopropene and anhydrous potassium carbonate is 1:1.2:1.5. After dripping, the temperature is gradually raised to 80°C, refluxed, reacted for 48h, filtered, and the solvent is removed under reduced pressure distillation, and a small amount of water is added Dilute and extract with ethyl acetate and saturated brine. Combine the organic phases, add anhydrous sodium sulfate, let stand overnight, collect by dry silica gel method, use a mixed solvent of petroleum ether / ethyl acetate (volume ratio 4:1) as the eluent for chromatographic column separation, vacuum at 50°C Af...
Example Embodiment
[0089] Example 3
[0090] The allylation reaction of 3-methyl-4-hydroxybenzaldehyde monomer, the reaction equation is as follows:
[0091]
[0092] Experimental steps:
[0093] Add 3-methyl-4-hydroxybenzaldehyde (10 mmol) to the flask and dissolve it in 30 ml of absolute ethanol, add anhydrous potassium carbonate (15 mmol), stir at room temperature for 30 min, and gradually under nitrogen atmosphere Add bromopropene (12 millimoles) dropwise, the molar ratio of syringaldehyde to bromopropene to anhydrous potassium carbonate is 1:1.2:1.5. After the addition, the temperature is gradually raised to 80°C, refluxed, reacted for 48h, filtered, The solvent was removed under reduced pressure distillation, diluted with a small amount of water, and extracted with ethyl acetate and saturated brine. Combine the organic phases, add anhydrous sodium sulfate, let stand overnight, collect by dry method on silica gel, use a mixed solvent of petroleum ether / ethyl acetate (volume ratio 10:1) as the el...
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