反应详情

Pyridine (100 mL) was cooled to 0° C., and N,O-dimethylhydroxylamine hydrochloride (20.14 g, 206 mmol) was added with stirring. This solution was stirred for 10 minutes, and then a solution of butyryl chloride (19.5 ml, 20 g, 188 mmol) dissolved in 50 ml methylene chloride was added via addition funnel over 30 minutes. A precipitate formed after 5 minutes. This suspension was stirred and allowed to warm to room temperature. Stirring was continued for 2.0 hours, and the reaction was diluted with water, extracted with methylene chloride twice. The methylene chloride layers were combined and washed with 1 N HCl twice and once with brine. Diethyl ether (100 mL) was added to facilitate emulsion separation, and the organic layer was separated and washed with saturated bicarbonate solution, brine, and dried over magnesium sulfate. The solution was filtered and the solvent removed in vacuo to give N-Methoxy-N-methyl-butyramide as an oil (22.1 g, 89%).

1. stirringThis solution was stirred for 10 minutes
2. additionwas added via addition funnel over 30 minutes
3. customA precipitate formed after 5 minutes
4. stirringThis suspension was stirred
5. stirringStirring
6. extractionextracted with methylene chloride twice
7. washwashed with 1 N HCl twice
8. additionDiethyl ether (100 mL) was added
9. customemulsion separation
10. customthe organic layer was separated
11. washwashed with saturated bicarbonate solution, brine
12. dry with materialdried over magnesium sulfate
13. filtrationThe solution was filtered
14. customthe solvent removed in vacuo