Method for synthesizing guaiacyl glycerol-beta-guaiacyl ether from lignin beta-O-4 linkage dimer model compound
A technology of wood-based glycerol and dimer, which is applied in the preparation of carbon-based compounds, organic compounds, and condensation to prepare carbonyl compounds. It can solve the problems of not getting high-value utilization and burning, and achieve high yield , short production cycle and simple method
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Embodiment 1
[0053] 1. Synthesis of 4-acetylguaiacol
[0054] (1) 85% phosphoric acid of 100.0g is poured in the eggplant-shaped bottle that the anhydrous phosphorus pentoxide of 122.0g is housed, heat and stir at 100 ℃ on oil bath for 1 hour, form polyphosphoric acid (PPA);
[0055] (2) 8.0g anhydrous sodium acetate is added in the round-bottomed flask that fills 15.0g guaiacol, mix well, the liquid in the eggplant-shaped bottle in (1) is poured in the round-bottomed flask while hot, and in Stir vigorously at 100°C for 10 minutes; place the reacted mixture in an ice-water bath to cool, then add sufficient distilled water and stir to dissolve it. Then extract with dichloromethane until the dichloromethane layer is colorless. After drying the extract with anhydrous sodium sulfate, evaporate the dichloromethane under reduced pressure to obtain dark red crystals; dissolve the product in a small amount of ethanol and heat to 80°C , and then add a few drops of distilled water to the position w...
Embodiment 2
[0068] 1. Synthesis of 4-acetylguaiacol
[0069] (1) 85% phosphoric acid of 120.0g is poured in the eggplant-shaped bottle that the anhydrous phosphorus pentoxide of 140.0g is housed, heat and stir at 100 ℃ on oil bath for 2 hours, form polyphosphoric acid (PPA);
[0070] (2) 12.0g anhydrous sodium acetate is added in the round-bottomed flask that fills 20.0g guaiacol, mix well, the liquid in the eggplant-shaped bottle in (1) is poured in the round-bottomed flask while hot, and in Stir vigorously at 100°C for 20 minutes; place the reacted mixture in an ice-water bath to cool, then add sufficient distilled water and stir to dissolve it. Then extract with dichloromethane until the dichloromethane layer is colorless. After drying the extract with anhydrous sodium sulfate, evaporate the dichloromethane under reduced pressure to obtain dark red crystals; dissolve the product in a small amount of ethanol and heat to 80°C , and then add a few drops of distilled water to the position...
Embodiment 3
[0083] 1. Synthesis of 4-acetylguaiacol
[0084] (1) 85% phosphoric acid of 100.0g is poured in the eggplant-shaped bottle that the anhydrous phosphorus pentoxide of 144.0g is housed, heat and stir at 100 ℃ on oil bath for 3 hours, form polyphosphoric acid (PPA);
[0085] (2) 12.0g anhydrous sodium acetate is added in the round-bottomed flask that fills 40.0g guaiacol, mix well, the liquid in the eggplant-shaped bottle in (1) is poured in the round-bottomed flask while hot, and in Stir vigorously at 100°C for 20 minutes; place the reacted mixture in an ice-water bath to cool, then add sufficient distilled water and stir to dissolve it. Then extract with dichloromethane until the dichloromethane layer is colorless. After drying the extract with anhydrous sodium sulfate, evaporate the dichloromethane under reduced pressure to obtain dark red crystals; dissolve the product in a small amount of ethanol and heat to 80°C , and then add a few drops of distilled water to the position...
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