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
- 50 °C
PROCEDURE
实验过程
0.3 g of sodium hydride (60% suspension in paraffin oil) is introduced into 10 ml of THF and 0.5 mL [sic] of 2,5-dimethylpyrrole in 10 ml of THF is added dropwise (5 minutes). After stirring at 50° C. for 1 hour, a reddish suspension is present. 1.3 g of 5-bromobenzofuran-2-carbonyl chloride in 10 ml of THF is [sic] added dropwise at 25° C. (5 minutes) and the mixture is subsequently stirred for 2 hours. The addition of 100 ml of completely deionized water and 100 ml of ethyl acetate follows. The separated organic phase was additionally washed 2× with 100 ml of water and concentrated in vacuo. After chromatography on silica gel (eluent heptane/ethyl acetate 4:1), the residual oil gives 700 mg of yellow crystals (yield 44%), m.p. 115-116°.
WORKUP
后处理
- additionis added dropwise (5 minutes)
- additionadded dropwise at 25° C. (5 minutes)
- stirringthe mixture is subsequently stirred for 2 hours
- washThe separated organic phase was additionally washed 2× with 100 ml of water
- concentrationconcentrated in vacuo