反应详情

To a solution of the compound prepared in Example 68 (0.067 g, 0.084 mmol) in dichloromethane (2 mL) at 0° C. was added trifluoroacetic acid (0.09 mL, 1.2 mmol). The reaction was warmed to room temperature and stirred for 4 h whereupon the solvent and excess trifluoroacetic acid was removed in vacuo. The resulting residue was dissolved in methanol (5 mL) and 6 M hydrochloric acid (0.70 mL) was added. The mixture was concentrated to dryness and the process repeated twice. The residue was triturated with methanol and methyl tert-butyl ether, the resulting solids dissolved in water and lyophilized to afford the title compound (0.050 g, 96%) as a yellow solid.

1. customwas removed in vacuo
2. dissolutionThe resulting residue was dissolved in methanol (5 mL)
3. addition6 M hydrochloric acid (0.70 mL) was added
4. concentrationThe mixture was concentrated to dryness
5. customThe residue was triturated with methanol and methyl tert-butyl ether
6. dissolutionthe resulting solids dissolved in water