HRID31425
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
Phosphorousoxychloride (2 ml) was added to 1H-pyrrole-2-carboxylic acid, 1-methyl-2-(4-iodobenzoyl)hydrazide (Intermediate 39) (150 mg) in acetonitrile (1 ml) and the reaction heated at 100° C. for 18 hours. The cooled reaction was poured onto ice/water (60 ml) and extracted with ethyl acetate (3×40 ml). The combined extracts were reduced to dryness under vacuum and the residue applied to a bond-elut (silica) and eluted with an ethyl acetate/cyclohexane gradient to give, after evaporation of the solvent, 2-(4-iodophenyl)-5-(1-methyl-1H-pyrrol-2-yl)-1,3,4-oxadiazole.
WORKUP
后处理
- customThe cooled reaction
- additionwas poured onto ice/water (60 ml)
- extractionextracted with ethyl acetate (3×40 ml)
- washeluted with an ethyl acetate/cyclohexane gradient
- customto give
- customafter evaporation of the solvent, 2-(4-iodophenyl)-5-(1-methyl-1H-pyrrol-2-yl)-1,3,4-oxadiazole