HRID710243
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
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
- extractionthe aqueous phase re-extracted with ethyl acetate
- dry with materialThe combined organic layers were dried (MgSO4)
- customevaporated
- customThe residue was purified by flash chromatography (10 g silica gel, 10 to 20% ethyl acetate in heptane)