反应详情

温度

65 °C

A solution of 4-(7-bromo-3-oxo-2H-isoquinolin-2-ylmethyl)benzoic acid tert-butyl ester (1.50 g, 3.62 mmol) in dimethylformamide (10 mL) is degassed with nitrogen, then treated with triethyl-amine (2.07 mL, 14.8 mmol), CuI (0.050 g, 0.26 mmol), Pd(Ph3P)4 (0.173 g, 0.15 mmol), and 3-phenyl-1-propyne (1.13 mL, 9.05 mmol). The reaction mixture is heated in an oil bath at 65° C. for 5 hours, cooled to room temperature, the DMF is evaporated, and the residue is dissolved in ethyl acetate. The solution is washed with 1N HCl, brine, dried over MgSO4 and evaporated onto silica gel. Purification on a 3.5×18 cm silica gel column eluted with hexane/ethyl acetate 4:1, followed by drying, will afford the desired product.

1. temperaturecooled to room temperature
2. customthe DMF is evaporated
3. dissolutionthe residue is dissolved in ethyl acetate
4. washThe solution is washed with 1N HCl, brine
5. dry with materialdried over MgSO4
6. customevaporated onto silica gel
7. customPurification on a 3.5×18 cm silica gel column
8. washeluted with hexane/ethyl acetate 4:1
9. customby drying