反应详情

温度

-15 °C

A solution of the compound obtained in step h above (22h) (300 mg, 0.782 mmol), NMM (0.19 mL, 1.72 mmol) and HOBt (179 mg, 1.329 mmol) in DMF (11 mL) were stirred at 0° C. for 10 minutes, then the reaction was cooled to −15° C., and EDCI (165 mg, 0.860 mmol) was added. The reaction was stirred for 30 minutes at −15° C. and then allowed to warm to room temperature, BnONH2HCl (137 mg, 0.860 mmol) was added. After being stirred overnight, the reaction mixture was concentrated under vacuum, and the residue was diluted with EtOAc and washed with brine. The combined organic layers were dried and concentrated; the residue was purified by silica gel column chromatography which gave the title compound as colorless oil (426 mg, 83% yield).

1. temperatureto warm to room temperature
2. stirringAfter being stirred overnight
3. concentrationthe reaction mixture was concentrated under vacuum
4. additionthe residue was diluted with EtOAc
5. washwashed with brine
6. customThe combined organic layers were dried
7. concentrationconcentrated
8. customthe residue was purified by silica gel column chromatography which