反应详情

温度

90 °C

Diethyl cyanophosphonate 90% (1.3 mL, 8.4 mmol) was slowly added at 25° C. to a mixture of 4-Methylsulfanyl-[2,2′]bipyridinyl 1-oxide (650.0 mg, 2.98 mmol) and triethylamine (0.50 mL, 3.58 mmol) in acetonitrile (14 mL) and stirred for 2 hours at 90° C. The reaction mixture was concentrated under reduced pressure, methanol (5 mL) added and the solid formed filtered and washed with methanol (2×5 mL), the filtrate was concentrated and purified by column chromatography on silica gel (0 to 10% Methanol in dichloromethane) to afford 4-methylsulfanyl-[2,2′]bipyridinyl-6-carbonitrile as a white solid that was combined with the previous white solid obtained (500.0 mg, 74%).

1. concentrationThe reaction mixture was concentrated under reduced pressure, methanol (5 mL)
2. additionadded
3. customthe solid formed
4. filtrationfiltered
5. washwashed with methanol (2×5 mL)
6. concentrationthe filtrate was concentrated
7. custompurified by column chromatography on silica gel (0 to 10% Methanol in dichloromethane)