반응 #163998

반응 방정식

2-(2,3,3-Trimethyl-3H-indol-5-ylmethyl)-isoindole-1,3-dione

Ethanol

perchloric acid

→

5-(1,3-Dioxo-1,3-dihydro-isoindol-2-ylmethyl)-2,3,3-trimethyl-3H-indolium perchlorate

반응 조건

후처리

1. 1
   기타equipped with magnetic stir bar and a reflux condenser
2. 2
   온도with heating
3. 3
   온도under reflux until all solids
4. 4
   workup.DISSOLUTIONdissolved
5. 5
   여과the separated crystals were filtered
6. 6
   세척washed with cold ethanol (100 mL), diethyl ether (2*100 mL)
7. 7
   기타dried

실험 절차

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).

출처