HRID2068634
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
- 170 °C
PROCEDURE
实验过程
5-(2-Bromo-acetyl)-thiophene-3-carboxylic acid methyl ester (0.4 g, 1.52 mmol) was dissolved in formamide (2 mL) and the tube purged with nitrogen and then sealed. The mixture was heated at 170° C. for 20 minutes. The resultant solution was diluted with HCl (1 M) and water and washed with ethyl acetate. The organic phase was evaporated then purified by chromatography on a silica II cartridge, eluting with 2:1 pentane:DCM to neat DCM, to give the side product, 5-oxazol-4-yl-thiophene-3-carboxylic acid methyl ester as white solid (0.049 g). LCMS m/z 251.35 [M+MeCN+H]+ R.T.=3.07 min (Analytical Method 6).
WORKUP
后处理
- customthe tube purged with nitrogen
- customsealed
- additionThe resultant solution was diluted with HCl (1 M) and water
- washwashed with ethyl acetate
- customThe organic phase was evaporated
- customthen purified by chromatography on a silica II cartridge
- washeluting with 2:1 pentane