反应详情

Acetyl chloride (4 μL, 0.057 mmol) was added under nitrogen to a solution of 4 (38 mg, 0.051 mmol) and N,N′-diisopropylethylamine (DIPEA; 8.7 μL, 0.062 mmol) in CHCl3 (2 mL). After 12 h, the reaction mixture was successively partitioned between CHCl3 and diluted NaHCO3, dried (Na2SO4) and evaporated. The residue was purified by column chromatography to give 25 mg (61.7%) of the title product 5 as a white powder: m/z=782 (M+H)+. NMR (DMSO-d6): δ (ppm) 1.19-1.35 (m, 4H), 1.68-1.77 (m, 4H), 1.90 (m, 2H), 2.02 (s, 3H, COCH3), 2.18 (m, 2H), 2.33 (m, 2H), 2.50 (m, 1H), 2.75 (m, 2H), 2.92 (s, 3H, SO2CH3), 2.96 (m, 2H), 3.33 (m, 8H), 4.43 (s, 2H, CH2CONH), 5.22 (s, 2H, OCH2), 5.35 (m, 1H), 5.53 (m, 1H), 7.17-7.20 (m, 3H), 7.39-7.60 (m, 5H), 7.69-7.79 (m, 2H), 7.86 (broad s, 1H, NH), 8.33+8.56 (m, 1H, NH), 9.95 (s, 1H, NH).

1. customthe reaction mixture was successively partitioned between CHCl3 and diluted NaHCO3
2. dry with materialdried (Na2SO4)
3. customevaporated
4. customThe residue was purified by column chromatography