Hydrochloric Acid → HCID 59239640, compound

Participants

Reaction Steps

Step 2—Synthesis of compound um: (S)-Tert-butyl 2-(4-(1-methyl-2,6-dioxo-1,2,3,6-tetrahydropyrimidin-4-ylamino)phenyl)-4-(3-methylmorpholino)-5,6-dihydropyrido[3,4-d]pyrimidine-7(8H)-carboxylate (0.196 g, 0.000357 mol) and 4.0 M of Hydrogen chloride in 1,4-Dioxane (5.00 mL) were mixed and stirred for 2 hours. The mixture was concentrated, diluted with sat NaHCO3 and extracted three times with 10% MeOH in dichloromethane. The aqueous layer was lyophilized, slurried in MeOH, vacuum filtered, and purified by HPLC. 1H NMR (400 MHz, DMSO) δ 8.95 (s, 1H), 8.28 (d, J=8.7, 2H), 8.23 (s, 1H), 7.28 (d, J=8.7, 2H), 6.52 (s, 1H), 5.02 (s, 1H), 4.11 (d, J=6.4, 1H), 3.88 (d, J=11.1, 3H), 3.71 (dd, J=11.3, 2.8, 1H), 3.65-3.56 (m, 3H), 3.08 (s, 3H), 2.99-2.92 (m, 1H), 2.87-2.80 (m, 1H), 2.58 (s, 2H), 1.24 (d, J=6.6, 3H). LC/MS-m/z+450.2 (M+H)+

Provenance & Evidence