反应详情

温度

0 °C

In a 20 mL pear-shaped flask, (1S,9S)-tert-butyl 9-amino-6,10-dioxooctahydro-1H-pyridazino[1,2-a][1,2]diazepine-1-carboxylate (0.9 g, 3.03 mmol) was combined with DMF (8 ml) to give a colorless solution and cooled to 0° C. Sodium carbonate (385 mg, 3.63 mmol) and benzyl carbonochloridate (516 mg, 432 μl, 3.03 mmol) were added and stirred at room temperature for 6 hr. It was diluted with brine and H2O, extracted with EtOAc (2×60 ml). The combined organic layer was washed with brine and H2O, dried with MgSO4, filtered and concentrated in vacuo to afford (1S,9S)-tert-butyl-9-(benzyloxycarbonylamino)-6,10-dioxooctahydro-1H-pyridazino[1,2-a][1,2]diazepine-1-carboxylate as an oil (1.3 g, 99.5%). ESI-LRMS m/e calcd for C18H21N3O6 [M+] 431. found 432 [M+H+]. The crude was used without further purification.

1. customto give a colorless solution
2. extractionextracted with EtOAc (2×60 ml)
3. washThe combined organic layer was washed with brine and H2O
4. dry with materialdried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo