Synthesis method of p-acetoxystyrene
A technology of acetoxystyrene and acetoxyacetophenone, applied in the field of synthesis of p-acetoxystyrene, can solve the problems of low yield, high solvent recovery cost, large reaction system and the like, and achieves high yield , Reduce recycling costs and equipment costs, the effect of low three wastes
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Embodiment 1
[0034]Step A: The hydroxyacetophenone (200 g, 1.47 mol) was dissolved in 1 l of dichloromethane, and triethylamine (223 g, 2.20 mol) was added, cooled to 0 ° C, slowly drop with acetic anhydride with stirring (180g, 1.76mol), after the end of the drop, the temperature increased to 30 ° C for 3 hours, and 500 ml of water was added after the reaction was completed, and the organic phase and the aqueous phase were separated, and the aqueous phase was extracted three times with dichloromethane (200 mL × 3). The organic phase was concentrated, and the acetoxyphenylidene (238.7 g, yield was 91.2%).
[0035]Step B: PD / C (10 g) was added to 500 mL of methanol (100 g, 0.56 mol) in 500 ml of methanol, and pd / c (10g) was added to the hydrogen replacement protection, under a hydrogen atmosphere, 2MPa, 30 The reaction was reacted for 5 hours, the reaction was completed, and PD / C was filtered by diatomal soil, and the filtrate was directly concentrated to give 4-acetyloxyphenylmethyl methanol ...
Embodiment 2
[0038]Step C-2: 4-acetyloxyphenylmethyl methanol (50 g, 0.31 mol), 0.15 g phenothiazine and 1-hexyl-3-methylimidazolium chloride (200 g) were added to the reaction bottle, After 6 hours of reaction to 150 ° C, after the reaction, the reaction was extracted three times with toluene (100 × 3), and 1-hexyl-3-methylimidazolium chloride was recovered, and the organic phase was added to 100 ml of water washing, and the organic phase was added after separation. 5 g of sodium anhydrous sulfate was dried, and the crude product was concentrated in vacuo, and 0.1 g of phenothiazine was added, and the decompression was purified to give acetoxystyrene (37.3 g, 82.9%, purity 99.69%).
Embodiment 3
[0040]Step c-3: 4-acetyloxyphenylmethyl methanol (50 g, 0.31 mol), 0.15 g phenothiazine and 1-ethyl-3-methylimidazolium hydrogen sulfate (200 g) were added to the reaction bottle In the middle, heated to 150 ° C for 6 hours, after the reaction was completed, extracted three times with toluene (100 × 3), and recovered 1-ethyl-3-methylimidazolium hydrogen sulfate, the organic phase was added to 100 ml of water washing, separated After the addition of 5 g of 5 g of sodium anhydrous sulfate was dried, the crude product was concentrated in vacuo, and 0.1 g of phenothiazine was added, and the decompression was purified to give acetoxystyrene (40.5 g, 90.0%, purity 99.70%).
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