HRID982009

反应详情

EQUATION

反应方程式

HRID 982009 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5-bromoindole (6.6 g), N-methylethenesulphonamide (5.1 g) palladium (II) acetate (75 mg), tri-o-tolylphosphine (0.2 g), triethylamine (12 ml), and acetonitrile (5 ml) was heated at 100° in an autoclave for 3 h. The reaction mixture was cooled and partitioned between hydrochloric acid (1N, 300 ml) and ethyl acetate (2×150 ml). The combined extracts were dried, (Na2SO4) and evaporated in vacuo to give an oil which was purified by `flash` chromatography (Q, 7 cm dia. col.) to give the title compound as a solid (2.3 g) m.p. 164√-166°.

WORKUP

后处理

  1. temperaturewas heated at 100° in an autoclave for 3 h
  2. temperatureThe reaction mixture was cooled
  3. custompartitioned between hydrochloric acid (1N, 300 ml) and ethyl acetate (2×150 ml)
  4. customThe combined extracts were dried
  5. custom(Na2SO4) and evaporated in vacuo
  6. customto give an oil which
  7. customwas purified by `flash` chromatography (Q, 7 cm dia. col.)