反应详情

1.3 g (5.02 mmol) of 6-nitro-1-benzofuran-2-carboxylic acid, 1.0 g (5.02 mmol) of R-aminoquinuclidine dihydrochloride, 2.29 g (6.02 mmol) of HATU, 2.34 g (18.07 mmol) of N,N-diisopropylethylamine and 10 ml of DMF are reacted by general method B. The mixture is concentrated in vacuo and extracted with 1 N sodium hydroxide solution and with ethyl acetate, the organic phase is dried over sodium sulfate and concentrated, and the residue is dissolved in methanol. Dowex 50WX2-200 ion exchanger resin is added, and within 1 h, the mixture is concentrated in a rotary evaporator. The resin is washed successively with methanol, DMF, methanol, THF, methanol, dichloromethane, methanol and 10% triethylamine in methanol. The product fraction is concentrated. 1.75 g (99% of theory) of the title compound are obtained.

1. concentrationThe mixture is concentrated in vacuo
2. extractionextracted with 1 N sodium hydroxide solution and with ethyl acetate
3. dry with materialthe organic phase is dried over sodium sulfate
4. concentrationconcentrated
5. dissolutionthe residue is dissolved in methanol
6. additionDowex 50WX2-200 ion exchanger resin is added
7. concentrationthe mixture is concentrated in a rotary evaporator
8. washThe resin is washed successively with methanol, DMF, methanol, THF, methanol, dichloromethane, methanol and 10% triethylamine in methanol
9. concentrationThe product fraction is concentrated