HRID982005

反应详情

EQUATION

反应方程式

HRID 982005 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe resulting cooled mixture
  2. customwas partitioned between hydrochloric acid (2N, 300 ml) and ethyl acetate (2×150 ml)
  3. dry with materialThe combined extracts were dried (Na2SO4)
  4. customevaporated in vacuo
  5. customThe residue was purified by `flash` chromatography (V, 7 cm col.)