HRID1897497

反应详情

EQUATION

反应方程式

HRID 1897497 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated under reduced pressure
  3. dissolutiondissolved in dichloromethane (20 mL)
  4. washThe solution was washed with water (3×10 mL), brine (10 mL)
  5. dry with materialdried over MgSO4
  6. filtrationfiltered through Celite
  7. concentrationconcentrated under reduced pressure
  8. customThe tan oil was chromatographed
  9. washeluting with ether