反应详情

(3S,4S)-4-[(S)-3-(4-fluorobenzyl)-piperidin-1-ylmethyl]-1,1-dioxo-tetrahydrothiophen-3-ylamine (47 mg, 137 μmol) and (2-morpholin-4-yl-ethyl)-carbamic acid 4-nitro-phenyl ester hydrochloride (55 mg, 164 μmol) were dissolved in N,N-dimethylformamide (1 mL) and treated with triethylamine (23 μL, 164 μmol). The mixture was stirred at room temperature for 67 h , and then concentrated. The residue was purified by flash column chromatography (3% methanol/dichloromethane containing 0.3% aqueous ammonium hydroxide). After isolation, the product was dissolved in 1N hydrochloric acid and water and lyophilized to provide a fluffy white solid (70 mg, 90%). 1H NMR (300 mHz, CD3OD) δ7.15 (m, 2H), 6.98 (m, 2H), 4.21 (q, J=8.1 Hz, 1H), 3.68 (m, 4H), 3.49 (dd, J=13.6, 8.1 Hz, 1H), 3.35 (m, 1H), 3.25 (t, J=6.6 Hz, 2H), 2.98 (m, 2H), 2.78 (m, 2H), 2.6-2.4 (11H), 2.07 (m, 1H), 1.9-1.5 (5H), 0.98 (m, 1H), ESI MS: (M+H)+=497.1.

1. concentrationconcentrated
2. customThe residue was purified by flash column chromatography (3% methanol/dichloromethane containing 0.3% aqueous ammonium hydroxide)
3. dissolutionAfter isolation, the product was dissolved in 1N hydrochloric acid