反应详情

温度

0 °C

A mechanically-stirred mixture of tert-butyl thiomorpholine-4-carboxylate (243 g, 1.19 mol), MeOH (1.5 L), and H2O (1.5 L) was cooled to 0° C. Solid NaIO4 (280 g, 1.3 mol) was added in portions over a 2 hour period. For convenience, the suspension was stirred for 3 days at room temperature. The solids were filtered, washing with MeOH (3×500 mL). The filtrate was concentrated. Residual water was saturated with solid NaCl, and the aqueous phase was extracted with EtOAc (4×200 mL). The combined organic phases were dried (MgSO4), filtered, and concentrated to obtain the product (255 g, 97%).

1. filtrationThe solids were filtered
2. washwashing with MeOH (3×500 mL)
3. concentrationThe filtrate was concentrated
4. extractionthe aqueous phase was extracted with EtOAc (4×200 mL)
5. dry with materialThe combined organic phases were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated