反应详情

温度

0 °C

A solution of 3-(aminomethyl)pyridine (12 μl, 0.11 mmol) in 0.5 ml of nitromethane was cooled to -20° C. and treated with 0.23 ml (0.12 mmol) of a 0.5M solution of carbonyl bis (N-methyl) imidazole triflate (Rappoport, et. al., J. Am. Chem. Soc. 1989, 111, 6856) in nitromethane. After 30 min, the solution was treated with a solution of 50 mg (0.08 mmol) of the resultant compound of Example 240 in 1.0 ml of dimethylformamide and 26 μL. (0.24 mmol) of 4-methylmorpholine. The resulting solution was stirred at 0° C. for 1 h, concentrated in vacuo, partitioned between chloroform and aqueous NaHCO3, dried over Na2SO4, and concentrated. The residue was purified by silica gel chromatography using 3% methanol in chloroform to provide 40 mg (65%) of the desired compound (Rf 0.4, 10% methanol in chloroform) as a white solid, m.p. 205°-206° C. Mass spectrum: (M+H)+ =737.

1. concentrationconcentrated in vacuo
2. custompartitioned between chloroform and aqueous NaHCO3
3. dry with materialdried over Na2SO4
4. concentrationconcentrated
5. customThe residue was purified by silica gel chromatography