反应详情

温度

22 °C

Intermediate 12 (0.050 g) was treated with N,N-dimethylformamide (0.5 ml) followed by 1-hydroxybenzotriazole hydrate (0.027 g), 1-[3-(dimethylamino)propyl]-3-ethylcarbodiimide hydrochloride (0.044 g) and Intermediate 1 (0.042 g) in N,N-dimethylformamide (0.5 ml) and N,N-diisopropylethylamine (0.027 ml). The mixture was stirred at 22° C. for 20 h, then left to stand for 6 days. The solution was diluted with dichloromethane (10 ml) and washed successively with dilute aqueous sodium hydrogen carbonate (10 ml) and dilute aqueous sodium chloride (2×10 ml). The organic phase was isolated using a hydrophobic frit (6 ml) and drained directly onto an SCX column (2 g Isolute SPE) which had been prepared by application of methanol. Elution with methanol, then 0.880 ammonia:methanol 10:90 gave the title compound (0.048 g) as an orange glassy solid.

1. waitleft
2. waitto stand for 6 days
3. washwashed successively with dilute aqueous sodium hydrogen carbonate (10 ml) and dilute aqueous sodium chloride (2×10 ml)
4. customThe organic phase was isolated
5. washElution with methanol