反应详情

温度

80 °C

To a solution of (ACY) (0.78 mmol) in dry DMF (5 mL) was added triethylamine (0.94 mmol), followed by 2-bromoacetamide (0.27 mmol). The resulting mixture was heated at 80° C. overnight. After completion of the reaction, the cooled mixture was partitioned between ether and brine, and the organic phase was separated, dried (MgSO4), and the solvent removed at the rotary evaporator to yield a pale yellow gum. Flash chromatography (SiO2, ether:methanol:ammonium hydroxide (1000:4:1)) gave compound (ACZ) as a white solid. (48% yield). Compound (ACZ): purity >97% (HPLC); MS: m/z 506.2 (M+1); 1H NMR (DMSO d6): δ 1.8 (m, 2H), 2.2 (m, 4H), 2.6-2.8 (m, 6H), 5.35 (s, 2H), 7.0-7.5 (m, 16H), 7.7 (m, 1H).

1. customAfter completion of the reaction
2. customthe cooled mixture was partitioned between ether and brine
3. customthe organic phase was separated
4. dry with materialdried (MgSO4)
5. customthe solvent removed at the rotary evaporator
6. customto yield a pale yellow gum