反应详情

Into a 1000-mL round-bottom flask was placed a solution of diethyl 2-(2-cyanovinylamino)malonate (30 g, 119.3 mmol, 1.00 equiv, 90%) in ethanol (420 mL) and sodium ethanolate (80 mL, 21%). The resulting solution was stirred for 3 days at room temperature. After the addition of acetic acid (15 ml), the resulting mixture was concentrated under vacuum, dissolved in 200 mL of dichloromethane, washed with 2×100 mL of saturated aqueous sodium bicarbonate and 1×100 mL of brine, dried over anhydrous sodium sulfate and concentrated. The residue was dried in HV to afford 10 g (49%) of ethyl 3-amino-1H-pyrrole-2-carboxylate as an orange syrup.

1. customInto a 1000-mL round-bottom flask was placed
2. concentrationthe resulting mixture was concentrated under vacuum
3. dissolutiondissolved in 200 mL of dichloromethane
4. washwashed with 2×100 mL of saturated aqueous sodium bicarbonate and 1×100 mL of brine
5. dry with materialdried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was dried in HV