反应详情

Freshly distilled propionyl chloride (0.04 ml, 0.41 mmole) (the receptacle is fitted with a trap containing CaCl2) was added to a solution of amine 8a (0.10 g, 0.40 mmole) and triethylamine (0.04 ml, 0.38 mmole) in dichloromethane (5 ml) at 0° C. The mixture was agitated at ambient temperature for 5 hours. The solvent was evaporated, water was added and the solid was isolated by filtration. The residue was purified by column chromatography using a mixture of dichloromethane and ethanol (94:6) as eluant and at the end ethyl acetate in order to obtain the compound 11c (0.10 g, 90%) in the form of a white powder: melting point 186-188° C.; NMR-1H (DMSO-d6) δ 11.86 (1H, s, NH-1), 8.60 (1H, s, NH-3), 7.21 (1H, s, H-6), 6.88 (1H, s, H-4'), 6.80 (2H, s, H-2' and 6'), 4.04 (2H, q, J=7 Hz, COCH2CH3), 2.22 (6H, s, CH3 -3' and 5'), 1.82 (3H, s, CH3 -5), 1.20 (3H, t, J=7 Hz, COCH2CH3). Anal. C17H20N2O2S . 1.25H2O (C, H, N, S).

1. customThe solvent was evaporated
2. additionwater was added
3. customthe solid was isolated by filtration
4. customThe residue was purified by column chromatography
5. additiona mixture of dichloromethane and ethanol (94:6) as eluant