反应详情

温度

83 °C

Potassium carbonate (330 mg) and 1-bromo-2-chloroethane (0.2 mL) were added to a stirred solution of N-cyclopropyl-3-(3-(2-(2-hydroxyphenyl)propan-2-ylamino)-2-oxopyrazin-1(2H)-yl)-4-methylbenzamide (Example 134, 0.1 g) in acetonitrile (5 mL). The reaction mixture was stirred under nitrogen at 83° C. for 16 h then concentrated in vacuo. The residue was treated with water and extracted into dichloromethane. The organic phase was washed with brine, dried (Na2SO4), filtered and concentrated in vacuo. The residue (120 mg) was treated with 33% methylamine in ethanol (3 mL) and heated within a microwave at 100° C. for 60 minutes. The mixture was concentrated in vacuo. Purification by preparative HPLC (Gemini column, 0.1% ammonia:acetonitrile eluent) afforded the title compound as a solid (65 mg).

1. concentrationthen concentrated in vacuo
2. additionThe residue was treated with water
3. extractionextracted into dichloromethane
4. washThe organic phase was washed with brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. additionThe residue (120 mg) was treated with 33% methylamine in ethanol (3 mL)
9. temperatureheated within a microwave at 100° C. for 60 minutes
10. concentrationThe mixture was concentrated in vacuo
11. customPurification by preparative HPLC (Gemini column, 0.1% ammonia:acetonitrile eluent)