HRID1017728
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
- 0 °C
PROCEDURE
实验过程
A solution of ethyl azidoacetate (1.38 g) and thiophene-2-carboxaldehyde (1 g) in ethanol (20 ml) was added dropwise to a solution of potassium ethoxide (0.9 g) in ethanol (20 ml) at 0° C. The reaction was stirred for 2 hours at 0° C. and 2 hours at ambient temperature then poured into saturated aqueous ammonium chloride solution (150 ml) and extracted with ether. Combined organic extracts were dried (MgSO4), concentrated in vacuo and the residue purified by column chromatography using isohexane as eluent to give the product as a pale yellow crystalline solid (0.49 g, 25%), NMR d(CDCl3) 1.40 (3H, t), 4.37 (2H, q), 7.08 (2H, m), 7.18 (1H, s), 7.38 (1H, m), 7.52 (1H, d).
WORKUP
后处理
- extractionextracted with ether
- dry with materialCombined organic extracts were dried (MgSO4)
- concentrationconcentrated in vacuo
- customthe residue purified by column chromatography