反应详情

To a stirred solution of dimethylamine hydrochloride (153 g, 187 mmol) in DMF (8 mL) was added DIPEA (2 mL, 6.55 mmol), (S)-2-tert-butoxycarbonylamino-3-pyridin-2-ylpropionic acid (0.50 g, 1.87 mmol, Acros) and TBTU (0.60 g, 1.87 mmol). The reaction mixture was stirred at rt for 16 h. The solvent was removed in vacuo and the residue was dissolved in methanol (15 mL). To this was added 4M hydrochloric acid in dioxane (20 mL) and the reaction stiffed at rt for 16 h. The solvent was removed in vacuo and the residue partitioned between water (100 mL) and ethyl acetate (2×100 mL). The aqueous layer was evaporated to dryness to give a solid, which was recrystallised from ethanol to give the title compound as a pale brown solid. mr/z (ES+)=194.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in methanol (15 mL)
3. additionTo this was added 4M hydrochloric acid in dioxane (20 mL)
4. customthe reaction stiffed at rt for 16 h
5. customThe solvent was removed in vacuo
6. customthe residue partitioned between water (100 mL) and ethyl acetate (2×100 mL)
7. customThe aqueous layer was evaporated to dryness
8. customto give a solid, which
9. customwas recrystallised from ethanol