反应详情

温度

70 °C

A solution of crude 1-aminomethyl-cyclopentylamine (Intermediate J) (80 mg, 0.70 mmol) in propan-2-ol (1.0 ml) is added to a suspension of 1-(3,5-diamino-6-chloro-pyrazine-2-carbonyl)-2-methyl-isothiourea (Intermediate A) (208 mg, 0.54 mmol) in propan-2-ol (1.08 ml) and heated at 70° C. for 2 days. After cooling to room temperature, the reaction mixture is filtered under vacuum, and the solid is rinsed with MeOH. The filtrate is concentrated in vacuo to afford a bright yellow residue which is loaded onto a SCX-2 cartridge and eluted with 33% NH3 (4 drops) in MeOH (5 ml×2). The methanolic ammonia fractions are combined and concentrated in vacuo. Purification using mass directed preparative LCMS eluting with 95% Water+0.1% NH3: 5% Acetonitrile to affords the title compound; [M+H]+ 310.

1. temperatureAfter cooling to room temperature
2. filtrationthe reaction mixture is filtered under vacuum
3. washthe solid is rinsed with MeOH
4. concentrationThe filtrate is concentrated in vacuo
5. customto afford a bright yellow residue which
6. washeluted with 33% NH3 (4 drops) in MeOH (5 ml×2)
7. concentrationconcentrated in vacuo
8. customPurification
9. washeluting with 95% Water+0.1% NH3