Method for preparing 2,3-epoxypinane by epoxidation of alpha-pinene
A technology of pinane oxide and epoxidation, which is applied in the fields of chemical synthesis and perfume chemistry, can solve the problems of difficult separation, difficult recovery and recycling of homogeneous catalysts, and achieves low cost, high selectivity, safe and reliable process. Effect
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Embodiment 1
[0025] Add 5.0g Al 2 o 3 , 30g pinene, 60.0g each of acetone and acetonitrile as solvent, 0.2Mol / L NaHCO 3 Solution 80g, start stirring, control the temperature at 50°C, add 70.0g of 30% hydrogen peroxide within 10 hours through the dropping funnel, and recover Al by filtration after the reaction 2 o 3 , extract the organic phase, wash the organic phase with sodium hydroxide and sodium sulfate solution to neutrality respectively, recover the solvent, obtain 2,3-epoxy pinane after rectification under reduced pressure, and analyze the conversion of α-pinene by gas chromatography The yield was 96%, and the yield of pinane epoxy was 92%.
Embodiment 2
[0027] In a 500ml four-necked flask with a condenser, a stirrer, a thermometer and a dropping funnel, add 5.0g of SiO 2 , 40g pinene, each 70g of acetone 80g acetonitrile as solvent, the NaHCO of 0.5Mol / L 3 Solution 40g, start stirring, control the temperature at 55°C, add 80g of 35% hydrogen peroxide through the dropping funnel within 15 hours, and recover SiO2 by filtration after the reaction, extract the organic phase, and wash the organic phase with sodium hydroxide and sodium sulfate solution respectively. phase to neutral, recover the solvent, and then rectify under reduced pressure to obtain 2,3-epoxy pinane. According to gas chromatography analysis, the conversion rate of α-pinene is 100%, and the yield of epoxy pinane is 97%.
Embodiment 3
[0029] Add 5.0g of SnO to a 500ml four-neck flask with condenser, stirrer, thermometer and dropping funnel 2 , 40g pinene, 60g acetone, 80g acetonitrile as solvent, 1Mol / L NaHCO 3 Solution 30g, start stirring, control the temperature at 60°C, add 120g of 27.5% hydrogen peroxide within 10 hours through the dropping funnel, and recover SnO by filtration after the reaction is completed. 2 , extract the organic phase, wash the organic phase with sodium hydroxide and sodium sulfate solution to neutrality respectively, recover the solvent, obtain 2,3-epoxy pinane after rectification under reduced pressure, and analyze the conversion of α-pinene by gas chromatography The yield was 99%, and the yield of pinane epoxy was 94%.
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