反应详情

温度

40 °C

This material was then combined with 1H-benzo[d][1,2,3]triazol-1-ol (0.012 g), and triethylamine (0.0613 mL) in N,N-dimethylformamide (0.5 mL). 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide (0.0145 g) was then added to the reaction mixture. After stirring for 30 minutes, the compound prepared in Example 214 (0.030 g) was added to the reaction mixture. The reaction mixture was allowed to stir at room temperature for 3 hours. Equivalent amounts of 1H-benzo[d][1,2,3]triazol-1-ol, triethylamine, and the compound prepared in Example 214 were added to the reaction mixture, and then heated at 40° C. for 17 hours. The reaction mixture was diluted with saturated sodium hydrogen carbonate aqueous solution and extracted with ethyl acetate. The combined organics were then washed with water and brine, dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (dichloromethane:methanol=19:1) to obtain the title compound (0.0085 g) having the following physical data.

1. stirringto stir at room temperature for 3 hours
2. extractionextracted with ethyl acetate
3. washThe combined organics were then washed with water and brine
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated
6. customThe residue was purified by column chromatography on silica gel (dichloromethane:methanol=19:1)