反应详情

温度

0 °C

To Boc-Gly-OH (1 g, 5.71 mmol) in DCM (12 mL) under N2 atmosphere at 0° C. was added DMAP (1.743 g, 14.27 mmol) and Meldrum's acid (0.987 g, 6.85 mmol). A solution of isopropyl chloroformate (8.56 mL, 8.56 mmol) in toluene was added dropwise. The reaction mixture was stirred at 0° C. for 3 h. The reaction mixture was washed with 15% KHSO4 twice, dried over sodium sulfate, filtered and evaporated. The crude product was taken in 50 mL of EtOAc and refluxed for 1 h. After volatile materials were evaporated, the crude product was triturated with EtOAC and the resulting solid was filtered and dried to provide a yellow solid (75%). LCMS (m/z): 200.1 (MH+), 0.504 min.

1. washThe reaction mixture was washed with 15% KHSO4 twice
2. dry with materialdried over sodium sulfate
3. filtrationfiltered
4. customevaporated
5. temperaturerefluxed for 1 h
6. customAfter volatile materials were evaporated
7. customthe crude product was triturated with EtOAC
8. filtrationthe resulting solid was filtered
9. customdried