تفاعل #216635

معادلة التفاعل

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

1,2-ethanedithiol

boron trifluoride etherate

→

title compound

المردود 64.0%

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

المردود 64.0%

المذيبات

benzene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas refluxed for 23 hours
2. 2
   ترشيحthe precipitate was filtered off
3. 3
   غسيلwashed with benzene and water
4. 4
   أخرىdried
5. 5
   أخرىThe crude material (0.64 g) was recrystallized twice from ethanol

الإجراء التجريبي

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).

المصدر