反应详情

温度

79 °C

To a suspension of 5-bromo-benzothiazol-2-ylamine IV (0.23 g, 1.0 mmol) in 1,4-dioxane (10 mL) was added ethylisocyanate (0.36 g, 0.38 mL, 5.02 mmol). The reaction mixture was heated up to 78-80° C. overnight. After completion of reaction (TLC monitoring), 1,4-dioxane was distilled off and co evaporated with hexane. The resulting solid was treated with water to 60-70° C. for 3-5 h. The resulting solid was filtered off and again washed with hot water, dried under high vacuum to obtain the desired product as off-white solid (0.15 g, 50%). 1H NMR (DMSO-d6, 400 MHz): δ 1.08 (t, J=7.20 Hz, 3H), 3.18 (m, 2H), 6.70 (br s, 1H), 7.36 (dd, J=1.60 and 8.0 Hz, 1H), 7.79 (d, J=1.60 Hz, 1H), 7.84 (d, J=8.40 Hz, 1H) and 10.85 (br s, 1H). MS: 300.07 (M+H+).

1. distillationwas distilled off
2. customco evaporated with hexane
3. additionThe resulting solid was treated with water to 60-70° C. for 3-5 h
4. filtrationThe resulting solid was filtered off
5. washagain washed with hot water
6. customdried under high vacuum