反应详情

A solution of 3-(benzyloxy)-2-(5-(4-fluorobenzyl)thiazol-2-yl)-9,9-dimethyl-6,7-dihydropyrimido[2,1-c][1,4]oxazin-4(9H)-one (0.051 g, 0.11 mmol) in TFA (5 mL) was stirred 24 h at 40 C. Then, the reaction mixture was cooled, concentrated and purified by preparative HPLC on C18 column using water/MeOH containing 0.1% TFA as eluent to afford the title compound (0.033 g, 80% yield) as pale yellow solid. 1HNMR (500 MHz, CDCl3) δ: 11.51 (1H, s), 7.61 (1H, s), 7.22 (2H, dd, J=8.6, 5.5 Hz), 7.03 (2H, t, J=8.6 Hz), 4.17 (2H, s), 4.06-4.01 (4H, m), 1.60 (6H, s). HRMS (M+H) calcd for C19H19N3O3FS: 388.1131. found: 388.1118. Anal calcd for C19H18N3O3FS: C, 58.90; H, 4.68; N, 10.84. found: C, 58.87; H, 4.47; N, 10.87.

1. temperatureThen, the reaction mixture was cooled
2. concentrationconcentrated
3. custompurified by preparative HPLC on C18 column