反应详情

To the crude (1-benzyl-piperidin-3-yl)-phenyl-amine (164) (1.11 g) in CH2Cl2 (5 ml) at 0° C. was added i-Pr2NEt (1.45 ml) and propionyl chloride (0.54 ml). The mixture was stirred for 2 hr. The mixture was diluted with CH2Cl2 (20 ml), washed with sat. NaHCO3 (2×10 ml), brine (10 ml) and water (10 ml) and dried with Na2SO4. After filtration, the filtrate was concentrated under vacuum. The residue was purified by silica gel chromatography (0.5% to 2% MeOH in CH2Cl2) to give 165 as a colorless oil. LRMS (calculated for C21H26N2O) 322. found 322; IR (film) 3059, 2937, 2863, 2797, 1657, 1594, 1499, 1390, 1264, 1101, 1074, 739, 703 cm−1.

1. washwashed with sat. NaHCO3 (2×10 ml), brine (10 ml) and water (10 ml)
2. dry with materialdried with Na2SO4
3. filtrationAfter filtration
4. concentrationthe filtrate was concentrated under vacuum
5. customThe residue was purified by silica gel chromatography (0.5% to 2% MeOH in CH2Cl2)