反应详情

To a solution of 2-diethylamino-4-(4-fluoro-phenyl)-5,6,7,9-tetrahydro-pyrimido[4,5-c]azepine-8-carboxylic acid tert-butyl ester (0.058 g, 0.14 mmol) in EtOAc (1 mL) was added 4 M HCl in dioxane (2 mL). After 16 h, the mixture was concentrated, diluted with saturated (satd.) aqueous (aq.) NaHCO3, and extracted with CH2Cl2. The combined organic layers were dried and concentrated. Purification by FCC (2 M NH3 in MeOH/CH2Cl2) provided the title compound (>90%). HPLC: Rt=9.7 min. MS (ESI): mass calcd. for C18H23FN4, 314.4; m/z found, 315.4 [M+H]+. 1H NMR (CDCl3): 7.47 (dd, J=8.7, 5.5, 2H), 7.11 (t, J=8.7, 2H), 3.96 (5, 2H), 3.64 (q, J=7.0, 4H), 3.21-3.18 (m, 1H), 2.80-2.76 (m, 2H), 1.93-1.86 (m, 2H), 1.71-1.67 (m, 1H), 1.17 (t, J=7.0, 6H).

1. concentrationthe mixture was concentrated
2. additiondiluted with saturated (satd.) aqueous (aq.) NaHCO3
3. extractionextracted with CH2Cl2
4. customThe combined organic layers were dried
5. concentrationconcentrated
6. customPurification by FCC (2 M NH3 in MeOH/CH2Cl2)