反应详情

0.5 g of the compound prepared in Example 11 is dissolved in 34.6 ml of anhydrous tetrahydrofuran and 4 ml of dimethylformamide. 3.5 ml of water and 0.208 g of caesium carbonate are added and the reaction mixture is left at room temperature for 1 hour. It is concentrated under vacuum and treated azeotropically with toluene. The residue is taken up in 5 ml of tetrahydrofuran. 0.6 ml of methyl iodide is added and the reaction mixtureis left for 1 hour at room temperature. It is concentrated under vacuum, the residue is taken up in water, the mixture is stirred and the precipitate is separated by filtration. The precipitate is washed with water and with pentane.

1. concentrationIt is concentrated under vacuum
2. additiontreated azeotropically with toluene
3. addition0.6 ml of methyl iodide is added
4. waitthe reaction mixtureis left for 1 hour at room temperature
5. concentrationIt is concentrated under vacuum
6. customthe precipitate is separated by filtration
7. washThe precipitate is washed with water and with pentane