反应详情

The product from step c (823 mg, 4.39 mMol) and 3-(4-fluorophenyl)propylamine (674 mg, 4.39 mMol) were dissolved in anhydrous acetonitrile (10 ml). To this solution, lithium trifluoromethanesulfonate (1.44 g, 9.23 mMol) was added, and the solution was stirred overnight. The mixture was concentrated in-vacuo, then the residue was dissolved in EtOAc (60 ml), washed with saturated sodium bicarbonate (2×20 ml), followed by water (20 ml). The organic phase was dried over sodium sulfate and concentrated to a yellow oil. Purified via flash chromatography, eluting with EtOAc, 2.5% 7N NH4 in MeOH/EtOAc, 5% 7N NH4 in MeOH/EtOAc to yield 1.2 g of a colorless oil as product. ESI+MS detects 341 (M+H).

1. concentrationThe mixture was concentrated in-vacuo
2. dissolutionthe residue was dissolved in EtOAc (60 ml)
3. washwashed with saturated sodium bicarbonate (2×20 ml)
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated to a yellow oil
6. customPurified via flash chromatography
7. washeluting with EtOAc, 2.5% 7N NH4 in MeOH/EtOAc, 5% 7N NH4 in MeOH/EtOAc