反应详情

温度

120 °C

4-(3-(4-fluorophenyl)-1-methyl-1H-pyrazol-4-yl)-6-methyl-5H-pyrrolo[3,4-b]pyridine-5,7(6H)-dione (intermediate from Example 1, step 5, 190 mg, 0.588 mmol) and 28-30% aqueous ammonium hydroxide (4 mL) were heated to a vigorous reflux for 30 min and then concentrated. The residue was dissolved in 1:1 acetic acid/acetic anhydride (20 mL) and heated at 120° C. for 2 hr and concentrated. The residue was dissolve in EtOAc and run through a short silica gel plug to afford 176 mg (92%) of Ex 4-Step 1 product as a white solid which was used without further purification: LCMS m/z 323.1 (M+1); 1H NMR (400 MHz, CDCl3) δ 8.63 (d, J=5.2, 1H), 8.15 (s, 1H), 7.37 (dd, J=8.8, 5.5, 2H), 7.17 (d, J=5; 3, 1H), 7.04 (dd, J=8.6, 8.6, 2H), 4.01 (s, 3H).

1. temperaturea vigorous reflux for 30 min
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in 1:1 acetic acid/acetic anhydride (20 mL)
4. concentrationconcentrated
5. dissolutionThe residue was dissolve in EtOAc
6. customto afford 176 mg (92%) of Ex 4-Step 1 product as a white solid which
7. customwas used without further purification