反应详情

A stirred mixture of D17 (0.32 g, 1.5 mmole), 3-bromo-2,6-dimethylpyridine hydrochloride (Synthesis 1974, 4, 293; 0.37 g, 1.6 mmole), Na2CO3 (0.48 g, 5.6 mmole) and tetrakis(triphenylphosphine)palladium (0) (0.08 g, 0.07 mmole) in 50% DME/water (20 ml) was heated at reflux under argon for 18 h. The mixture was concentrated in vacuo to 50% volume, diluted with water (20 ml), washed with EtOAc (2×10 ml), acidified with 2M HCl to pH 4 and extracted with DCM (3×25 ml). The combined extract was dried and evaporated to dryness. The residue was triturated in Et2O to afford the title compound as a buff powder (0.29 g, 69%).

1. temperaturewas heated
2. temperatureat reflux under argon for 18 h
3. concentrationThe mixture was concentrated in vacuo to 50% volume
4. additiondiluted with water (20 ml)
5. washwashed with EtOAc (2×10 ml)
6. extractionextracted with DCM (3×25 ml)
7. extractionThe combined extract
8. customwas dried
9. customevaporated to dryness
10. customThe residue was triturated in Et2O