反应详情

7.68 g (23 mmol) of the compound from Example XXIII and 4.4 g (23 mmol) of cyclooctyl bromide are dissolved in 100 ml of dimethylformamide. 3.36 g (30 mmol) of potassium tertiary butoxide, dissolved in 30 ml of DMF, are added dropwise to this mixture at 0°-10° C. with stirring. The mixture is subsequently stirred at room temperature for a further two hours and then treated with 30 ml of 1N hydrochloric acid. The solvent is then evaporated in vacuo, the residue is taken up in 200 ml of dichloromethane and the dichloromethane solution is washed twice with 100 ml of water. After drying with sodium sulphate, it is concentrated to a small volume in vacuo and the residue is separated by column chromatography (silica gel 60, eluent: toluene/ethyl acetate=4:1).

1. additionare added dropwise to this mixture at 0°-10° C.
2. stirringThe mixture is subsequently stirred at room temperature for a further two hours
3. customThe solvent is then evaporated in vacuo
4. washthe dichloromethane solution is washed twice with 100 ml of water
5. dry with materialAfter drying with sodium sulphate, it
6. concentrationis concentrated to a small volume in vacuo
7. customthe residue is separated by column chromatography (silica gel 60, eluent: toluene/ethyl acetate=4:1)