HRID1897497
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
A mixture of (S)-2-tert-butoxycarbonylamino-4-iodobutyric acid methyl ester (0.200 g, 0.58 mmol), (2-methoxyethyl)-methylamine (0.062 g, 0.70 mmol), and triethylamine (0.41 mL, 2.9 mmol) in dioxane (1 mL) was stirred at 70° C. for 16 hours. The mixture was cooled to room temperature, concentrated under reduced pressure, and dissolved in dichloromethane (20 mL). The solution was washed with water (3×10 mL), brine (10 mL), dried over MgSO4, filtered through Celite, and concentrated under reduced pressure. The tan oil was chromatographed eluting with ether to provide 0.87 g of pale yellow oil (49% yield).
WORKUP
后处理
- temperatureThe mixture was cooled to room temperature
- concentrationconcentrated under reduced pressure
- dissolutiondissolved in dichloromethane (20 mL)
- washThe solution was washed with water (3×10 mL), brine (10 mL)
- dry with materialdried over MgSO4
- filtrationfiltered through Celite
- concentrationconcentrated under reduced pressure
- customThe tan oil was chromatographed
- washeluting with ether