反应详情

温度

100 °C

To 2-(6-fluoropyridin-3-yl)-5-methoxy-1,3-benzothiazole (59.2 mg, 0.227 mmol) was added methylamine in ethanol (8 M, 2 mL) and the reaction mixture was heated in a microwave oven at 100° C. for 5 min. Water and dichloromethane were added and the layers separated. The aqueous phase was extracted with dichloromethane (3×). The combined organic phases were washed with water, dried (MgSO4), filtered and the solvent removed in vacuo. The crude material was purified by column chromatography (heptane/EtOAc 60:40 to 50:50) to give the title compound (39 mg) as a pale yellow solid. 1H NMR δ ppm 8.68 (d, 1 H) 7.98 (dd, 1 H) 7.91 (d, 1 H) 7.50 (d, 1 H) 7.27 (q, 1 H) 7.01 (dd, 1 H) 6.59 (d, 1 H) 3.85 (s, 3 H) 2.86 (d, 3 H); MS m/z (M+H) 272.

1. customthe layers separated
2. extractionThe aqueous phase was extracted with dichloromethane (3×)
3. washThe combined organic phases were washed with water
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe solvent removed in vacuo
7. customThe crude material was purified by column chromatography (heptane/EtOAc 60:40 to 50:50)