反应详情

温度

70 °C

5-(5-Quinolyl)pyrazine-2,3-diamine. (3-Amino-6-(5-quinolyl)pyrazin-2-yl)[(4-methoxy phenyl)methyl]amine (see Example 1.B) (0.210 g, 0.588 mmol) was dissolved in trifluoroacetic acid/dichloromethane (2 mL:2 mL) with PS-thiophenol as a scavenger. The solution was heated to 70° C. in a sealed tube for two hours and then concentrated under reduced pressure and diluted with methanol. The methanol/product solution was filtered through a Phenomenex Strata-X-C solid phase extraction column to remove TFA. Additional water was added to the eluted compound to induce precipitation. The precipitate was filtered and dried under vacuum to afford the title compound (0.080 g, 57% yield). MS (ESI) m/z 238.1 [M+1]+.

1. concentrationconcentrated under reduced pressure
2. additiondiluted with methanol
3. filtrationThe methanol/product solution was filtered through a Phenomenex Strata-X-C solid phase extraction column
4. customto remove TFA
5. additionAdditional water was added to the eluted compound
6. customprecipitation
7. filtrationThe precipitate was filtered
8. customdried under vacuum