Ethanol → HCID 59239340, compound

Participants

Reaction Steps

Step 2—Synthesis of compound xk: 1-(2-aminopropyl)-3-(4-(4-morpholino-7-(pyrimidin-2-yl)-5,6,7,8-tetrahydropyrido[3,4-d]pyrimidin-2-yl)phenyl)thiourea (0.293 g, 0.000579 mol) in dry Ethanol (12.0 mL, 0.206 mol) was added Mercury(II) oxide (0.260 g, 0.00120 mol). The reaction mixture was stirred at room temperature for 8 hours. The reaction mixture was heated at 40° C. and stirred overnight. The reaction mixture was heated at 50° C. and stirred overnight. The reaction mixture was heated at 78° C. for 8 hours. The reaction mixture was cooled to room temperature and stirred for 6 days. The reaction mixture was heated at 78° C. for 8 hours. The reaction mixture was cooled to room temperature, filtered through celite, filtered through a disc filter, concentrated, and purified by HPLC. 1H NMR (400 MHz, DMSO) δ 8.43 (d, J=4.7, 2H), 8.17 (d, J=8.5, 2H), 7.01 (s, 2H), 6.69 (t, J=4.7, 1H), 6.32 (s, 2H), 4.80 (s, 2H), 3.98 (s, 2H), 3.82-3.70 (m, 5H), 3.46 (s, 5H), 2.92 (s, 1H), 2.75 (s, 2H), 1.15 (d, J=6.1, 3H). LC/MS-m/z+472.2 (M+H)+

Provenance & Evidence