反应详情

Synthesized according to the method used for COMPOUND 41 except that INTERMEDIATE 5a was used. The residue was purified by flash chromatography, eluting 25% methanol in dichloromethane, rising to 40% methanol in dichloromethane. The product was converted to the hydrochloride salt using 2M HCl in diethyl ether to give COMPOUND 65 as a colourless solid. Purity (HPLC): >99%; Optical purity (Chiral HPLC): >99%; 1H NMR (400 MHz, CD3OD) 1.06 (t, J=6.64 Hz, 3H), 1.19 (t, J=6.88 Hz, 3H), 2.61 (t, J=7.66 Hz, 2H), 2.56-2.67 (m, 4H), 2.95 (t, J=7.66 Hz, 2H), 3.18-3.26 (m, 6H), 3.45-3.53 (m, 2H), 4.41 (s, 1H), 7.13-7.16 (m, 2H), 7.19-7.24 (m, 6H), 7.30 (d, J=8.30 Hz, 2H), 7.52 (d, J=8.20 Hz, 2H), Found: C, 61.14; H, 6.86; N, 9.10. C31H38N4O2×2.9HCl×0.3H2O has C, 61.06; H, 6.86; N, 9.19%. [a]D20=−0.96 deg [c 0.73, MeOH].

1. customSynthesized
2. customThe residue was purified by flash chromatography
3. washeluting 25% methanol in dichloromethane