反应详情

254 mg of the compound from Example 21A (0.84 mol) are dissolved in 5 ml of DMF, and 549 mg of caesium carbonate (1.68 mol) and 190 μl of ethyl bromoacetate (281 mg, 1.68 mol) are added. The reaction mixture is stirred at room temperature overnight. 6 ml of water are added, and the mixture is extracted three times with dichloromethane. The combined organic phases are washed with saturated sodium chloride solution and dried over sodium sulphate. The solvent is removed in a rotary evaporator, and the residue is purified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→95:5). 254 mg (29% of theory) of the title compound are obtained.

1. extractionthe mixture is extracted three times with dichloromethane
2. washThe combined organic phases are washed with saturated sodium chloride solution
3. dry with materialdried over sodium sulphate
4. customThe solvent is removed in a rotary evaporator
5. customthe residue is purified by preparative HPLC (eluent: acetonitrile/water, gradient 20:80→95:5)