1489-97-0 1,4-二氧杂螺[4.5]癸烷-8-羧酸乙酯

运输信息：常温运输。危险描述：非危险化学品。

化学合成。

化学合成

合成路线 1（1. 合成：1489-97-0）

• 步骤: 将4-氧代-环己烷羧酸乙酯（52.8g，0.31mol）、乙二醇（67.4g，1.08mol）和对甲苯磺酸（0.7g）的甲苯（160ml）溶液在室温下搅拌；将仲丁二醇（1.08mol）和对甲苯磺酸（0.7g）加入到4-氧代-环己烷羧酸乙酯（0.31mol）的甲苯（160ml）溶液中，25℃下搅拌20小时。反应完成后，将反应溶液倒入乙醚（300ml）中，加入乙酸乙酯（300ml），分离有机相，依次用水、饱和NaHCO₃水溶液和NaCl溶液洗涤，用Na₂SO₄干燥，真空浓缩，得到产物。
• 条件: With toluene-4-sulfonic acid In toluene at 20 - 25℃; for 20 h; Reflux（部分步骤）
• 收率: 100%
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合成路线 2（2. 合成：1489-97-0）

• 步骤: 将8.5g（54.4mmol）4-环己烷羧酸乙酯、3.8ml（68.0mmol）乙二醇和1.1g（5.8mmol）对甲苯磺酸一水合物溶解在250ml甲苯中，回流18小时。反应完成后，减压浓缩，加入200ml 5%碳酸氢钠水溶液，用300ml乙醚萃取三次，醚层用硫酸钠干燥，减压浓缩，硅胶柱色谱纯化得到产物。
• 条件: With toluene-4-sulfonic acid In toluene for 18 h; Reflux
• 收率: 90%
• 参考文献: [1] Patent: EP2602261, 2013, A1; [2] 17159-79-4; [3] 107-21-1; [4] 1489-97-0