反应详情

温度

-10 °C

2-(2,3,3-Trimethyl-3H-indol-5-ylmethyl)-isoindole-1,3-dione (126 g, 0.396 mol; Sigma-Aldrich) was placed in 1 L one-necked flask equipped with magnetic stir bar and a reflux condenser. 500 mL Ethanol (500 mL, 8 mol; Pharmco) were added to the flask followed by addition of perchloric acid (35 mL, 0.40 mol; Aldrich). The reaction mixture was stirred with heating under reflux until all solids dissolved. The solution was then cooled at −10° C. for 3 hours and the separated crystals were filtered, washed with cold ethanol (100 mL), diethyl ether (2*100 mL) and dried. The yield was 166 g (100% of theoretical).

1. customequipped with magnetic stir bar and a reflux condenser
2. temperaturewith heating
3. temperatureunder reflux until all solids
4. dissolutiondissolved
5. filtrationthe separated crystals were filtered
6. washwashed with cold ethanol (100 mL), diethyl ether (2*100 mL)
7. customdried