反应详情

温度

120 °C

A mixture of 5-chloro-7-morpholin-4-ylthiazolo[5,4-d]pyrimidine (3.0 g, 11.7 mmol), 2-ethylbenzimidazole (1.88 g, 12.9 mmol), tris(dibenzylideneacetone)dipalladium (534 mg, 0.60 mmol), XPhos (1.11 g, 2.34 mmol) and Cs2CO3 (7.62 g, 23 4 mmol) in dioxane (60 mL) was purged with argon then heated at 120° C. for 16 h in a sealed tube. The reaction mixture was filtered through Celite®, and the filtrated partitioned between EtOAc and H2O. The organic phase was washed with brine, then dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, EtOAc:DCM, 0-90%) followed by recrystallisation from iPrOAc affording the title compound (3.17 g, 74%). LCMS (method A): RT 2.74 min [M+H]+ 367.1

1. customwas purged with argon
2. filtrationThe reaction mixture was filtered through Celite®
3. customthe filtrated partitioned between EtOAc and H2O
4. washThe organic phase was washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated in vacuo
7. customThe resulting residue was purified by column chromatography (Si—PCC, EtOAc:DCM, 0-90%)
8. customfollowed by recrystallisation from iPrOAc affording the title compound (3.17 g, 74%)
9. customRT 2.74 min [M+H]+ 367.1