反应详情

温度

0 °C

To a solution of 4A (289 mg, 0.362 mmol) in dichloromethane (5 mL) and acetonitrile (5.00 mL) at 0° C., was added phosgene (20% in toluene) (0.242 mL, 0.488 mmol). The reaction mixture was stirred at 0° C. for 15 min. Nitrogen was bubbled though the mixture for 0.5 h, then DMPU (˜0.4 mL) was added. The resulting solution was added dropwise via a syringe pump into a solution of TEA (0.353 mL, 2.53 mmol) in dichloromethane (90 mL) at rt over 4 h, stirred for an additional 15 min and then evaporated. The crude product was purified by flash chromatography to give 4B (177 mg, 0.215 mmol, 59.3% yield) as a white solid. MS and 1H NMR are consistent with the desired product.

1. customNitrogen was bubbled though the mixture for 0.5 h
2. additionDMPU (˜0.4 mL) was added
3. stirringstirred for an additional 15 min
4. customevaporated
5. customThe crude product was purified by flash chromatography