反应详情

温度

25 °C

To a suspension of 5.0 g. (16.1 mmoles) of 1-ethyl-5-(2-carboxybenzyloxy)oxindole in 100 ml. of methylene chloride was added 3.34 g. (16.1 mmoles) of phosphorous pentachloride and the reaction mixture allowed to stir 30 minutes at 25° C. The reaction mixture was cooled to -15° C. and 8.56 g. (64.4 mmoles) of aluminum chloride was added. The resulting mixture was allowed to stir at room temperature for 30 minutes and was then added to ice. The organic phase was separated, dried over magnesium sulfate and concentrated to give the desired product which was recrystallized from ethyl acetate-hexane, 2.3 g (69% yield), m.p. 186.5°-188.5° C.

1. additionTo a suspension of 5.0 g
2. temperatureThe reaction mixture was cooled to -15° C.
3. stirringto stir at room temperature for 30 minutes
4. additionwas then added to ice
5. customThe organic phase was separated
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated