HRID982009
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
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
- temperaturewas heated at 100° in an autoclave for 3 h
- temperatureThe reaction mixture was cooled
- custompartitioned between hydrochloric acid (1N, 300 ml) and ethyl acetate (2×150 ml)
- customThe combined extracts were dried
- custom(Na2SO4) and evaporated in vacuo
- customto give an oil which
- customwas purified by `flash` chromatography (Q, 7 cm dia. col.)