反应详情

温度

170 °C

6-Methoxy-1,3-benzothiazole (0.100 g, 0.61 mmol) and 5-bromo-N-methylpyrimidin-2-amine (0.171 g, 0.91 mmol) were reacted according to the procedure used for the preparation of 2-(2-methoxypyrimidin-5-yl)-1,3-benzothiazole with the exception that the reaction was heated at 170° C. in a microwave reactor for 1.5 h. The reaction mixture was diluted with EtOAc and water and the mixture was filtered. The phases were separated and the aqueous layer was extracted with EtOAc (3×). The organic phase was washed with brine (2×), dried (MgSO4) and concentrated under vacuum. Flash chromatography (Heptane/EtOAc gradient) gave the title compound (54 mg) as a yellow solid. 1H NMR (CHLOROFORM-d) δ 8.93 (s, 2H) 7.91 (d, 1H) 7.35 (d, 1H) 7.10 (dd, 1H) 5.53 (br s, 1H) 3.90 (s, 3H) 3.11 (d, 3H); MS m/z (M+H) 273.

1. filtrationthe mixture was filtered
2. customThe phases were separated
3. extractionthe aqueous layer was extracted with EtOAc (3×)
4. washThe organic phase was washed with brine (2×)
5. dry with materialdried (MgSO4)
6. concentrationconcentrated under vacuum