反应详情

To a solution of BOC-L-Gln (20 g, 81 mmol) in 50 mL of EtOAC and MeOH at 0° C. was added diazomethane in 250 mL of Et2O with stirring. The resulting yellow solution was stirred at 0° C. for 5 minutes and then warmed up to room temperature and stirred for 20 minutes. Argon gas was then bubbled through the yellow reaction mixture to remove excess diazomethane. The crude product was concentrated and purified by crystallization from methyl-tert-butyl ether. Yield 100%. 1H NMR (CDCl3) δ 1.45 (s, 9H), 1.96 (m, 1H), 2.21 (m, 1H), 2.36 (m, 2H), 3.76 (s, 3H), 4.34 (m, 1H), 5.32 (m, 1H), 5.44 (bs, 1H), 6.16 (bs, 1H). Anal. (C11H20N2O5) C, H, N.

1. stirringThe resulting yellow solution was stirred at 0° C. for 5 minutes
2. stirringstirred for 20 minutes
3. customArgon gas was then bubbled through the yellow reaction mixture
4. customto remove excess diazomethane
5. concentrationThe crude product was concentrated
6. custompurified by crystallization from methyl-tert-butyl ether