反应详情

温度

100 °C

A glass microwave reaction vessel was charged with 5-bromo-3-iodo-1-(tetrahydro-2H-pyran-2-yl)-1H-indazole (2.04 g, 5.01 mmol), Pd(PPh3)4 (0.555 g, 0.480 mmol), CuI (0.130 g, 0.683 mmol) and 2-(methylthio)-4-(tributylstannyl)pyrimidine (2.23 g, 5.37 mmol, Frontier Scientific). DMF (6 mL) was added and the reaction mixture was sealed under argon and heated thermally at 100° C. for 6.5 h. The solvent was removed in vacuo and the residue was dissolved in MeOH, evaporated onto silica gel and purified by flash chromatography (Isco, (80 gram)) eluting with 2M NH3 in MeOH:DCM (0:1→1:19) to give 855 mg of a tan amorphous solid. m/z: 405.0 [M+1].

1. customA glass microwave reaction vessel
2. customthe reaction mixture was sealed under argon
3. customThe solvent was removed in vacuo
4. dissolutionthe residue was dissolved in MeOH
5. customevaporated onto silica gel
6. custompurified by flash chromatography (Isco, (80 gram))
7. washeluting with 2M NH3 in MeOH:DCM (0:1→1:19)