反应详情

To a 3-necked RBF (round bottomed flask) is added dichloromethane (2.4 L), (S)-4-benzyl-2-oxazolidinone (200 g, 1.13 moles) and N,N-Dimethyl-4-pyridinamine, (13.6 g; 111.32 mmoles). The flask is cooled in an ice water bath and triethylamine (472 mL; 3.39 moles) is added dropwise at 0° C. To the resulting solution is then added dropwise butanoyl chloride (152.2 mL; 1.46 moles) over 3 h, while keeping the temperature below 5° C. The reaction is then filtered and the filtrate is washed with 1M HCl (aq.) (500 ml×1) and saturated NaHCO3 (500 ml×1). The organic phase is dried over Na2SO4, filtered, and concentrated to afford the title compound (275 g, MS:[M+H]+=248.1 m/z).

1. temperatureThe flask is cooled in an ice water bath
2. customthe temperature below 5° C
3. filtrationThe reaction is then filtered
4. washthe filtrate is washed with 1M HCl (aq.) (500 ml×1) and saturated NaHCO3 (500 ml×1)
5. dry with materialThe organic phase is dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated