反应详情

温度

85 °C

6-(2-Methoxyphenyl)-2-(methylsulfinyl)pyrimidine-4-carboxamide (46 mg, 0.15 mmol), 1,4-dioxane (2 mL), DIPEA (80 μL, 0.45 mmol), and dimethylamine hydrochloride (26 mg, 0.3 mmol) were added to a vial (8 mL). The vial was sealed and heated at 85° C. for two days. After the reaction solution cooled to room temperature, the solvent was removed under vacuum in a Savant SpeedVac. The resulting residue was purified by Prep. HPLC. 1H NMR (300 MHz, CDCl3) δ 7.95 (q, J=7.8, 1.8 Hz, 1H), 7.88 (s, 1H), 7.77 (bs, 1H), 7.40 (m, 1H), 7.04 (t, J=9.0 Hz, 1H), 6.98 (d, J=6.0 Hz, 1H), 5.78 (bs, 1H), 3.92 (s, 3H), 3.26 (s, 6H). HPLC ret. time 2.76 min, 10-100% CH3CN, 5 min gradient; ESI-MS m/z 273.1 (M+H)+.

1. customThe vial was sealed
2. temperatureAfter the reaction solution cooled to room temperature
3. customthe solvent was removed under vacuum in a Savant SpeedVac
4. customThe resulting residue was purified by Prep
5. customHPLC ret. time 2.76 min, 10-100% CH3CN, 5 min gradient