反应详情

A solution of ethyl isonipecotate (4.9 mL, 31.8 mmol) and pyridine (2.8 mL, 34.6 mmol) was cooled to 0° C. Methanesulfonyl chloride (2.7 mL, 34.9 mmol) was added. After 1.5 hours, the reaction mixture was diluted with CH2Cl2 (300 mL) and extracted with saturated aqueous NaHCO3 (3×100 mL). The organic layer was dried over Na2SO4, filtered, and concentrated. The crude material was dissolved in EtOAc (400 mL), extracted with H2O (3×50 mL), dried over Na2SO4, filtered, and concentrated to give the pure product (5.42 g, 22.9 mmol, 72%) as a yellow solid. IR(CHCl3): 3027, 1726, 1331, 1158, 963.

1. extractionextracted with saturated aqueous NaHCO3 (3×100 mL)
2. dry with materialThe organic layer was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. dissolutionThe crude material was dissolved in EtOAc (400 mL)
6. extractionextracted with H2O (3×50 mL)
7. dry with materialdried over Na2SO4
8. filtrationfiltered
9. concentrationconcentrated