反应详情

温度

80 °C

A solution of 3-chloromethyl-1-methyl-1H-1,2,4-triazole (from Example 1, Step c; 600 mg, 4.6 mmol) in 40% aqueous methylamine and 1,4-dioxane (5 ml) was stirred and heated at 80° C. in a sealed tube for 16 hours. Upon cooling the whole mixture was evaporated (azeotroping with ethanol). The residue was purified by chromatography on silica gel, eluting with dichloromethane-methanol-aqueous ammonia (60:8:1→40:8:1) to give the title compound (440 mg, 80%) as a pale yellow oil. 1H NMR (250 MHz, d6-DMSO) δ 3.61 (2H, s), 3.81 (3H, s), 8.35 (1H, s); MS (ES+) m/e 127 [MH]+.

1. temperatureUpon cooling the whole mixture
2. customwas evaporated
3. custom(azeotroping with ethanol)
4. customThe residue was purified by chromatography on silica gel
5. washeluting with dichloromethane-methanol-aqueous ammonia (60:8:1→40:8:1)