13096-62-3 2,3,4,6-四苄基-D-吡喃葡萄糖酸-1,5-内酯

• [1] Bioorganic and Medicinal Chemistry Letters, 2012, vol. 22, # 1, p. 642 - 644 [2] Organic Process Research and Development, 2014, vol. 18, # 1, p. 66 - 81 [3] Patent: US2005/209166, 2005, A1. Location in patent: Page/Page column 26 [4] Patent: WO2006/138163, 2006, A2. Location in patent: Page/Page column 25-26

合成路线 3（3. 合成：13096-62-3）

产率：98% 合成条件：With acetic anhydride In dimethyl sulfoxide at 20℃; for 10 h; 实验步骤：向内酯17（37.4g，68.8mmol）在（195mL，2.75mol）DMSO中的溶液中将溶液在室温下搅拌20分钟，然后加入乙酸酐（130mL，1.37mol）。 在环境温度下搅拌10小时后，通过加入冷（0℃）淬灭溶液。 H2O（500mL）加完后，将溶液逐渐升至室温。 分离有机层，水层用EtOAc萃取。 将合并的有机层用盐水洗涤，用无水Na 2 SO 4干燥，过滤并真空浓缩。 通过硅胶柱色谱法（EtOAc-石油醚= 1:20）纯化得到的粗残余物，得到标题化合物（36.4g，98％），为无色油状物。 1H NMR（400MHz，CDCl3）δ7.40-7.17（m，20H），5.00（d，J = 11.2Hz，1H），4.76-4.45（m，8H），4.14（d，J = 6.4Hz，1H） ，3.98-3.90（m，2H），3.72-3.64（m，2H）。 参考文献：

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