反应详情

To a stirred solution of 4-phenylpyridine N-oxide (25 g, 0.146 mmol) in dichloromethane (200 ml) at room temperature was added trimethylsilyl cyanide (17.4 g), followed by the slow addition of dimethyl carbamyl chloride (16.2 ml) in dichloromethane (50 ml) over a 30 minute period. The reaction mixture was stirred at room temperature for one day, and then to it potassium carbonate solution (10%,150 ml) was added slowly. Stirring continued for an additional 30 minutes, the organic layer was separated, and the aqueous layer was extracted with dichloromethane. The extracts were combined and dried over magnesium sulfate. Evaporation in vacuo gave a crude reaction product (35 g) as a white solid. It was used without further purification.

1. stirringStirring
2. waitcontinued for an additional 30 minutes
3. customthe organic layer was separated
4. extractionthe aqueous layer was extracted with dichloromethane
5. dry with materialdried over magnesium sulfate
6. customEvaporation in vacuo
7. customgave a crude
8. customIt was used without further purification