HRID982005
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
- 100 °C
PROCEDURE
实验过程
A mixture of 5-bromoindole (7.7 g), N,N-dimethylethenesulphonamide (5.3 g) triethylamine (15 ml), acetonitrile (5 ml), palladium (II) acetate (0.35 g) and tri-o-tolylphosphine (0.95 g) was heated at 100° C. in an autoclave for 3 h. The resulting cooled mixture was partitioned between hydrochloric acid (2N, 300 ml) and ethyl acetate (2×150 ml). The combined extracts were dried (Na2SO4) and evaporated in vacuo. The residue was purified by `flash` chromatography (V, 7 cm col.) to give the title compound as a crystalline solid (3.8 g) m.p. 148°-150° C.
WORKUP
后处理
- temperatureThe resulting cooled mixture
- customwas partitioned between hydrochloric acid (2N, 300 ml) and ethyl acetate (2×150 ml)
- dry with materialThe combined extracts were dried (Na2SO4)
- customevaporated in vacuo
- customThe residue was purified by `flash` chromatography (V, 7 cm col.)