反应详情

A solution of tert-butyl 2-(4-(6-(4-chlorophenyl)-4-oxothieno[3,2-d]pyrimidin-3(4H)-yl)-2-methoxyphenoxy)acetate Example 14 (370 mg; 0.741 mmol) in 1:1 TFA/CH2Cl2 (6 mL) was stirred at rt for 1 h. After concentration under reduced pressure and azeotroping with toluene, the residue was triturated with MeOH to afford the title compound (290 mg; 88%) as a white solid. 1H NMR (DMSO-d6) δ 3.79 (s, 3H), 4.75 (s, 2H), 6.99-7.04 (m, 2H), 7.22 (d, J=2.20 Hz, 1H), 7.57 (d, J=8.80 Hz, 2H), 7.91 (d, J=8.25 Hz, 2H), 7.97 (s, 1H), 8.40 (s, 1H), 13.06 (s, 1H); 13C NMR (DMSO-d6) δ 55.76, 64.86, 111.95, 112.70, 119.41, 121.70, 121.98, 127.83, 129.26, 130.21, 131.18, 134.26, 147.36, 148.80, 149.44, 149.79, 156.06, 157.39, 169.9; HPLC (Method #1): 3.44 min retention time; MS (ES): m/z 443 [M+H]+.

1. concentrationAfter concentration under reduced pressure
2. customazeotroping with toluene
3. customthe residue was triturated with MeOH