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林产化学与工业 ›› 2007, Vol. 27 ›› Issue (S1): 77-80.

• 研究报告 • 上一篇    下一篇

桦木醇丁二酸酯的合成

田水清, 吕坤, 方桂珍, 韩世岩, 艾青   

  1. 东北林业大学 生物质材料科学与技术教育部重点实验室, 黑龙江 哈尔滨 150040
  • 收稿日期:2007-06-20 修回日期:1900-01-01 出版日期:2007-10-20 发布日期:2007-10-20
  • 通讯作者: 方桂珍,教授,博士生导师,主要从事木材化学和木材功能性改良方面的研究和教学工作;E-mail:fanggz@public.hr.hl.cn。

Synthesis of 3,28-Di-O-succinyl-betulin

TIAN Shui-qing, Lü Kun, FANG Gui-zhen, HAN Shi-yan, AI Qing   

  1. Key Laboratory of Bio-based Material Science and Technology, Northeast Forestry University, Ministry of Education, Harbin 150040, China
  • Received:2007-06-20 Revised:1900-01-01 Online:2007-10-20 Published:2007-10-20

摘要: 通过对桦木醇的C-3位、C-28位羟基进行修饰,在吡啶作溶剂,二甲基氨基吡啶(DMAP)作催化剂的条件下,与丁二酸酐反应合成桦木醇丁二酸酯.通过单因素试验,考察了物料比和反应时间对桦木醇丁二酸酯纯度的影响.确定合成反应的最佳条件:反应温度95℃,物料比(物质的量之比)1:18,反应时间10 h.对产物采用FT-IR、1H NMR和MS进行分析,确证桦木醇丁二酸酯的结构,并利用HPLC对产物含量进行分析,纯度为81.854%,得率为70.43%.

关键词: 桦木醇, 桦木醇丁二酸酯, 酯化反应

Abstract: Two acyl groups were respectively introduced at C-3 and C-28 hydroxyl groups of betulin. 3,28-di-O-succinyl-betulin was synthesized with pyridine as solvent and dimethylaminopyridine (DMAP) as catalyst from betulin and succinyl anhydride. The influences of the ratio of betulin to succinyl anhydride and reaction time on the purity of 3,28-di-O-succinyl-betulin were studied. The qualitative analysis was studied by FT-IR,1H NMR and MS.The quantitative analysis was examined by HPLC. The results showed that the optimal condition was as follows: molar ratio of betulin to succinyl anhydride 1 to 18, reaction temperature 95℃ and reaction time 10 h. The yield was 70.43% and the purity was 81.854% under these conditions.

Key words: betulin, 28-di-O-succinyl-betulin, esterification

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