反应详情

温度

50 °C

To a suspension of methanesulfinic acid sodium salt (310 mg, 3.04 mmol) in dry DMF (3.5 mL) was added under a nitrogen atmosphere, dry pyridine (0.5 mL) and 2-bromo-N,2-dimethylpropanamide (365 mg, 2.027 mmol). The reaction mixture was stirred at 50° C. overnight, cooled and H2O (5 mL) and EtOAc (10 mL) were added. The aqueous layer was separated and extracted twice with EtOAc (5 mL). The combined organic phase was washed with brine (20 mL) and dried over Na2SO4. The solution was concentrated in vacuo and stirred in heptane (25 mL). The solids were filtered to give the desired product (88 mg, 23%) as a white solid.

1. additionwas added under a nitrogen atmosphere
2. temperaturecooled
3. customThe aqueous layer was separated
4. extractionextracted twice with EtOAc (5 mL)
5. washThe combined organic phase was washed with brine (20 mL)
6. dry with materialdried over Na2SO4
7. concentrationThe solution was concentrated in vacuo
8. stirringstirred in heptane (25 mL)
9. filtrationThe solids were filtered