反应详情

温度

16 °C

A slurry of N-Boc-L-asparagine (5.00 g, 21.5 mmol), EtOAc (24 mL), acetonitrile (24 mL), water (12 mL), and PIDA (8.32 g, 25.8 mmol) was cooled and stirred at 16° C. for 30 min. The temperature was then allowed to reach 20° C., and the reaction was stirred until completion (ca. 4 h). The mixture was cooled to 0° C. and filtered. The filter cake was washed with EtOAc (10 mL) and dried in vacuo to give 1 (2.73 g, 62% yield). 1H NMR (CD3OD and a drop of TFA) δ4.05 (1H), 3.20-3.08 (2H), 1.45 (9H).

1. customto reach 20° C.
2. stirringthe reaction was stirred until completion (ca. 4 h)
3. temperatureThe mixture was cooled to 0° C.
4. filtrationfiltered
5. washThe filter cake was washed with EtOAc (10 mL)
6. customdried in vacuo