反应详情

温度

80 °C

A mixture of 1-(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-2-methyl-isothiourea (Intermediate A) (1.7 g, 4.54 mmol) and 4-aminomethyl-1-(1-phenyl-ethyl)-piperidin-4-ylamine (Intermediate BM) (1.6 g, 4.59 mmol) in propan-2-ol (50 ml) is stirred at 80° C. for 16 hours. The reaction mixture is concentrated in vacuo and purified by column chromatography (basic alumina, 0-2% MeOH in DCM) to obtain pale yellow solid. The compound obtained is further dissolved in MeOH and precipitated by adding diethyl ether. The supernatant solvent mixture is decanted and the product is washed again with diethyl ether and dried under vacuum to afford the title compound as off-white solid; [M+H]+ 429

1. concentrationThe reaction mixture is concentrated in vacuo
2. custompurified by column chromatography (basic alumina, 0-2% MeOH in DCM)
3. customto obtain pale yellow solid
4. customThe compound obtained
5. customprecipitated
6. additionby adding diethyl ether
7. customThe supernatant solvent mixture is decanted
8. washthe product is washed again with diethyl ether
9. customdried under vacuum