反应详情

温度

110 °C

Methyl 1-((ethoxycarbonyl)amino)-3-phenyl-1H-pyrrole-2-carboxylate (1.00 g, 3.47 mmol) was taken in a pressure tube and ammonium hydroxide (30%, 67.5 mL, 1.73 mol) was added and sealed. The reaction mixture was stirred at 110° C. for 30 h and transferred to a round bottomed flask and concentrated under reduced pressure. Toluene was added to it and azeotroped to remove trace amount of water (3 times). Then residue obtained was triturated with ethyl acetate (50×2 mL) to afford 5-phenylpyrrolo[2,1-f][1,2,4]triazine-2,4(1H,3H)-dione (0.300 g, 38.1%). LCMS Condition B-39: retention time 1.49 min, [M+1]=228.0.

1. customsealed
2. customtransferred to a round bottomed flask
3. concentrationconcentrated under reduced pressure
4. additionToluene was added to it
5. customazeotroped
6. customto remove trace amount of water (3 times)
7. customThen residue obtained
8. customwas triturated with ethyl acetate (50×2 mL)