반응 #216635

반응 방정식

9H-indeno[1,2-b]pyrazine-3,9(4H)-dione

1,2-ethanedithiol

boron trifluoride etherate

→

title compound

수율 64.0%

9H-Indeno[1,2-b]pyrazine-3,9(4H)-dione 9-ethylene dithioacetal

수율 64.0%

용매

benzene

반응 조건

후처리

1. 1
   온도was refluxed for 23 hours
2. 2
   여과the precipitate was filtered off
3. 3
   세척washed with benzene and water
4. 4
   기타dried
5. 5
   기타The crude material (0.64 g) was recrystallized twice from ethanol

실험 절차

A suspension of 9H-indeno[1,2-b]pyrazine-3,9(4H)-dione (0.50 g, 2.52 mmol) in benzene (10 ml), 1,2-ethanedithiol (0.63 ml, 7.56 mmol) and boron trifluoride etherate (0.31 ml, 2.52 mmol) was refluxed for 23 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with benzene and water and dried. The crude material (0.64 g) was recrystallized twice from ethanol to give 0.44 g (64%) of the title compound. M.p. 284°-290° C. 1H-NMR (DMSO-d6, δ): 3.75-3.94 (m, 4H), 7.46-7.57 (m, 2H), 7.8 (m, 2H), 7.95 (s, 1H), 12.6 (s, 1H).

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