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林产化学与工业

林产化学与工业 ›› 2009, Vol. 29 ›› Issue (6): 25-28.

• 研究报告 • 上一篇    下一篇

固体超强酸催化β-蒎烯合成龙脑研究

刘永根1, 陈慧宗2, 杨义文3   

  1. 1. 海南医学院药学系, 海南 海口 571101;2. 江西师范大学化学化工学院, 江西 南昌 330027;3. 嘉兴学院 生物与化学工程学院, 浙江 嘉兴 314001
  • 收稿日期:2008-11-15 修回日期:1900-01-01 出版日期:2009-12-30 发布日期:2009-12-30

Synthesis of Borneol from β-Pinene Catalyzed by Solid Superacid

LIU Yong-gen1, CHEN Hui-zong2, YANG Yi-wen3   

  1. 1. Department of Medicine, Hainan Medical College, Haikou 571101, China;2. Institute of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang 330027, China;3. School of Biology and Chemical Engineering, Jiaxing University, Jiaxing 314001, China
  • Received:2008-11-15 Revised:1900-01-01 Online:2009-12-30 Published:2009-12-30

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摘要： 在固体超强酸催化作用下β-蒎烯和无水草酸平稳地发生酯化反应,生成草酸龙脑酯;加入氢氧化钠溶液发生皂化反应得到龙脑。酯化反应采用程序升温的方式(65℃、1 h, 75℃、4 h, 90℃、1 h),皂化反应时间为 1 h。在上述反应条件下,当催化剂SO42-/ZrO2用量为 7% 时(以β-蒎烯质量计,下同),粗龙脑产率为 62.0%,产品中正、异龙脑比为13.6:48.7;当催化剂S2O82-/ZrO2用量为 7% 时,粗龙脑产率为 66.7%,正、异龙脑比为11.5:49.5;这两种催化剂对正龙脑选择性比较差。当用稀土复合固体超强酸SO42-/ZrO2-CeO2为催化剂,用量 3% 时,粗龙脑产率为 56.1%,但对正龙脑的选择性高于其他催化剂,正、异龙脑比为46.0:23.2。

关键词: 合成龙脑, β-蒎烯, 固体超强酸, 酯化-皂化法

Abstract: Bornyl oxalate was formed smoothly by esterification of β-pinene with anhydrous oxalic acid using solid superacid as catalyst. Borneol was obtained by saponification of bornyl oxalate with NaOH solution. Esterification was conducted by temperature programming method (65℃ 1h, 75℃ 4h, 90℃1 h)and the time of saponification was 1 h. When the amount of SO42-/ZrO2 catalyst was 7% of the mass of β-pinene, the yield of product was 62.0%,and the mass ratio of borneol to isoborneol in the product was 13.6:48.7. When the amount of S2O82-/ZrO2 catalyst was 7% of the mass of β-pinene, the yield of product was 66.7%,the mass ratio of borneol to isoborneol in the product was 11.5:49.5. Both two catalysts were poor for borneol selectivity. The yield of product was 56.1% when rare-earth composite solid superacid SO42-/ZrO2-CeO2 was used as catalyst at dosage of 3% of the mass of β-pinene, while mass ratio of borneol to isoborneol in the product reached 46.0:23.2, showing higher borneol selectivity than other catalysts.

Key words: synthetic borneol, β-pinene, nanometer solid super acid, esterification-saponification method

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