HRID710243

反应详情

EQUATION

反应方程式

HRID 710243 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

(S)-tert-Butyl 2-(4-formylphenyl)morpholine-4-carboxylate (120 mg, 0.41 mmol) was dissolved in methanol (5 ml), then potassium carbonate (114 mg, 0.824 mmol) was added, followed by dimethyl 1-diazo-2-oxopropylphosphonate (99 mg, 0.515 mmol). The mixture was stirred for 2 h at room temperature. Ethyl acetate (50 ml) and sodium bicarbonate solution (50 ml) were added, the aqueous phase re-extracted with ethyl acetate. The combined organic layers were dried (MgSO4) and evaporated. The residue was purified by flash chromatography (10 g silica gel, 10 to 20% ethyl acetate in heptane) to yield a colorless oil (103 mg, 87%).

WORKUP

后处理

  1. extractionthe aqueous phase re-extracted with ethyl acetate
  2. dry with materialThe combined organic layers were dried (MgSO4)
  3. customevaporated
  4. customThe residue was purified by flash chromatography (10 g silica gel, 10 to 20% ethyl acetate in heptane)