反应详情

温度

25 °C

A mixture of aqueous hydrochloric acid (34.5% w/w) (2.3 g) and methanol (20 ml) was added to a mixture of (1S,3S,5S)-2-[(2S)-2-tritylamino-2-(3-hydroxyadamantan-1-yl)acetyl]-2-azabicyclo[3.1.0]hexane-3-carbonitrile (10.0 g) in methanol (80 ml), and the mass was stirred at 25° C. for 3 hours. Completion of the reaction was verified by HPLC. Solvent was distilled from the reaction mixture to give a residue. Ethyl acetate (100 ml) was mixed with the residue for 30 minutes at ambient temperature. The solid was filtered and washed with ethyl acetate (2×5 ml). The solid was dried under vacuum at 50-60° C. for 8 hours to give the title product (6.0 g). (Yield=90%; HPLC purity=99.5%)

1. distillationSolvent was distilled from the reaction mixture
2. customto give a residue
3. filtrationThe solid was filtered
4. washwashed with ethyl acetate (2×5 ml)
5. customThe solid was dried under vacuum at 50-60° C. for 8 hours