تفاعل #160848

معادلة التفاعل

potassium carbonate

EtOH

1-amino-1H-pyrrole-2,4-dicarbonitrile

formamidine acetate

→

above compound

المردود 75.3%

4-aminopyrrolo[2,1-f][1,2,4]triazine-6-carbonitrile

المردود 75.3%

المذيبات

EtOAc

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةUpon cooling to rt
2. 2
   أخرىtransferred to a separatory funnel
3. 3
   غسيلwashed with water
4. 4
   أخرىThe organic layer was collected
5. 5
   تجفيفdried (MgSO4)
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated to dryness
8. 8
   أخرىThe crude material was then triturated with EtOH-water
9. 9
   أخرىThe solid was collected
10. 10
    غسيلwashed with water
11. 11
    أخرىdried under vacuum

الإجراء التجريبي

To a solution of EtOH (50 mL) was added 1-amino-1H-pyrrole-2,4-dicarbonitrile (1.00 g, 7.57 mmol) followed by formamidine acetate (9.46 g, 90.8 mmol) and potassium carbonate (14.6 g, 106.0 mmol). The solution was heated to 80° C. for 2 h. Upon cooling to rt, the reaction mixture was diluted with EtOAc transferred to a separatory funnel and washed with water. The organic layer was collected, dried (MgSO4), filtered, and concentrated to dryness. The crude material was then triturated with EtOH-water. The solid was collected, washed with water, and dried under vacuum to afford 0.91 g of the above compound as a yellow-orange solid (5.70 mmol, yield 75%). 1H-NMR (DMSO-d6) δ 8.37 (d, J=1.8 Hz, 1H), 8.19 (d, J=17.4, 2H), 7.93 (s, 1H), 7.27 (d, J=1.8 Hz, 1H); LCMS RT=1.14 min.

المصدر