تفاعل #216636

معادلة التفاعل

H2O

1,2-ethanedithiol

boron trifluoride etherate

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

→

title compound

المردود 83.0%

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

المردود 83.0%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe precipitate was filtered off
2. 2
   غسيلwashed with toluene, ethanol-water (2:1) and ethanol
3. 3
   أخرىThe crude material (2.40 g) was recrystallized from DMF-water

الإجراء التجريبي

A suspension of 9H-indeno[1,2-b]pyrazine-2,3,9(1H, 4H)-trione. 0.9 H2O (2.0 g, 8.68 mmol) in toluene (50 ml), 1,2-ethanedithiol (2.19 ml, 26.04 mmol) and boron trifluoride etherate (1.07 ml, 8.68 mmol) was refluxed for 20 hours. The reaction mixture was cooled to room temperature, and the precipitate was filtered off and washed with toluene, ethanol-water (2:1) and ethanol. The crude material (2.40 g) was recrystallized from DMF-water to give 2.09 g (83%) of the title compound. M.p. >300° C. 1H-NMR (DMSO-d6, δ): 3.68 (m, 2H), 3.91 (m, 2H), 7.2 (t, 1H), 7.3 (t, 1H), 7.51 (d, 1H), 7.59 (d, 1H), 12.05 (s, 1H), 12.38 (s, 1H).

المصدر