反应详情

温度

100 °C

1-(Dimethylamino)propan-2-ol (187 mg, 1.81 mmol) was added to a stirred suspension of sodium hydride (123 mg, 60% in mineral oil, 1.81 mmol) in 1,4-dioxane. After 30 minutes, 5-amino-3-chloropyrazine-2-carbonitrile (140 mg, 0.906 mmol) was added. The vial was capped and the reaction mixture was heated to 100° C. overnight. The reaction mixture was concentrated, diluted with methanol and adsorbed onto an SPE (TsOH) cartridge (pre-conditioned with methanol). The cartridge was rinsed with methanol and the product was eluted with 2 M NH3 in methanol. The basic fractions were concentrated to give the title compound as an orange oil which was used without further purification (79.2 mg, 0.358 mmol, 40%). LC-MS (1) Rt=1.33 m/z (ESI+) 222 (MH+).

1. customThe vial was capped
2. concentrationThe reaction mixture was concentrated
3. additiondiluted with methanol
4. washThe cartridge was rinsed with methanol
5. washthe product was eluted with 2 M NH3 in methanol
6. concentrationThe basic fractions were concentrated