紫苏醛的合成

Synthesis of Perillyl Aldehyde

研究以天然β-蒎烯为原料经化学合成制得紫苏醛。采用乙腈为介质,以氯化亚铜-苯甲酸铜为催化剂,β-蒎烯与过氧化苯甲酰在65±2℃反应16h,得到的紫苏醋酸酯进一步水解、水汽蒸馏得粗品,减压精馏得纯度为96%的紫苏醇,收率为73%;紫苏醇在二氯乙烷中,用K2S2O8-NaOH-H2O,在40℃催化氧化反应9h,经酸化、静置分层、水洗、干燥、回收溶剂后得紫苏醛,GC分析含量91.2%,收率85.5%。合成紫苏醛的总收率62%(以-β蒎烯计)。经分析测试证明产物与文献报道值相符。

The manufacture of perillyl alcohol from β-pine was investigated in 62% yield.To a mixture of β-pine 0.2mol,benzoyl peroxide 0.1mol,CuCl（0.2g）,cupric benzoate（1.5g） was added to acetonitrile（150mL） and the mixture was stirred for 16h at 65±2℃. Removal of the β-pine at 400Pa gave a residue benzoate ester on hydrolyzing in CH3OH-NaOH ,steam distilling gave a residue perillyl alcohol, and distillation under the vacuum gave the perillyl alcohol in 73%, and yielded a purity of 96%; In CH3ClCH3Cl, perillyl aldehyde was synthesized with perillyl alcohol, K2S2O8-NaOH-H2O and catalyst for 9h at 40℃,the organic layer was washed with H2O and dried with Na2SO4. Removal of the solevent gave perillyl aldehyde in 85.5%, and yielded a purity of 91.2%.