反应详情

A 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer was charged with 199c (7.0 g, 20.2 mmol, 1.0 eq.), triethylamine (4.08 g, 40.4 mmol, 2.0 eq.), and THF (50 mL). To the mixture was added the solution of acetyl chloride (2.36 g, 30.3 mmol, 1.5 eq.) in THF (20 mL) dropwise. The reaction mixture was stirred at room temperature for one hour. After the reaction was completed, it was quenched with ice water and evaporated under reduced pressure. The residue was extracted with dichloromethane. The combined organic layer was dried over Na2SO4 and concentrated under reduced pressure. The resulting residue was washed with 1:8 ethyl acetate/petroleum to afford 199d as a white solid (5.9 g, 76%). MS-ESI: [M+H]+ 388.3.

1. customA 250-mL single-neck round-bottomed flask equipped with a magnetic stirrer
2. customit was quenched with ice water
3. customevaporated under reduced pressure
4. extractionThe residue was extracted with dichloromethane
5. dry with materialThe combined organic layer was dried over Na2SO4
6. concentrationconcentrated under reduced pressure
7. washThe resulting residue was washed with 1:8 ethyl acetate/petroleum