反应详情

To a solution of 4-chloro-2-(N-cyanoamino)-6-[(4-methyl)-piperidin-1-yl]-5-phenylpyrimidine (0.1 g, 0.305 mmol) in dimethylformamide (4 ml) at room temperature was added water (2 ml) followed by potassium carbonate (0.084 g, 0.61 mmol) and the resulting suspension was warmed gently to afford a clear solution. To the cooled solution was then added methyl iodide (0.076 ml, 1.22 mmol) and the reaction mixture stirred at room temperature for 2.5 hours. The reaction was then quenched by the addition of saturated aqueous ammonium chloride solution (40 ml). After adding ethyl acetate (40 ml) the biphasic mixture was stirred for 5 minutes. The organic phase was then separated, washed with saturated brine (50 ml), dried over magnesium sulfate and concentrated in vacuo to afford a yellow syrup. The crude product was chromatographed an silica gel eluting with 90:10 v/v hexane: ethyl acetate to afford 0.09 g (87% yield) of the title compound as a colorless syrup.

1. temperaturethe resulting suspension was warmed gently
2. customto afford a clear solution
3. customThe reaction was then quenched by the addition of saturated aqueous ammonium chloride solution (40 ml)
4. additionAfter adding ethyl acetate (40 ml) the biphasic mixture
5. customThe organic phase was then separated
6. washwashed with saturated brine (50 ml)
7. dry with materialdried over magnesium sulfate
8. concentrationconcentrated in vacuo
9. customto afford a yellow syrup
10. customThe crude product was chromatographed an silica gel eluting with 90:10 v/v hexane