反应详情

To a solution of (3R,7S)-3-amino-1-cyclopentyl-7-phenyl-1,3,4,7-tetrahydro-2H-azepin-2-one (8f) (65 mg) in DCM (4 ml) at RT under N2 was added N-[(3,5-difluorophenyl)acetyl]-L-alanine (59 mg), HOBt (65 mg), EDAC.HCl (69 mg), and N-methylmorpholine (24 mg). The reaction was stirred at RT overnight, then diluted with DCM (10 ml) and washed with 1N HCl, 1N K2CO3, dried (Na2SO4), filtered and evaporated. The crude product was purified by flash chromatography (2% MeOH/DCM) to afford the title compound as an off white solid (60 mg, 50%). 1H NMR (300 MHz, CDCl3) δ 1.28 (d, 3H, J=7 Hz), 1.37-1.70 (m, 6H), 1.94-2.16 (m, 3H), 2.50-2.60 (m, 1H), 3.48 (s, 2H), 4.36-4.55 (m, 2H), 4.96 (d, 1H, J=8 Hz), 5.20 (tt, 1H, J=9 Hz, J=9 Hz), 5.87-5.94 (m, 1H), 6.18-6.33 (m, 2H), 6.67-6.80 (m, 3H), 7.00 (d, 1H, J=6 Hz), 7.25-7.38 (m, 5H). MS APCI, m/z=496 (M+1), LC/MS, 2.54 min.

1. washwashed with 1N HCl, 1N K2CO3
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. customevaporated
5. customThe crude product was purified by flash chromatography (2% MeOH/DCM)