反应详情

温度

60 °C

1.42 g (3.55 mmol) of the compound from Example 24A are initially charged in 30 ml of acetonitrile, 0.96 ml (7.10 mmol) of isopentyl nitrite and 0.95 g (7.10 mmol) of copper(II) chloride are added and the mixture is stirred at 60° C. for 5 hours. Once more, the same amount of copper(II) chloride is added and the mixture is stirred at 60° C. overnight. 7 ml of 1N hydrochloric acid are added, the mixture is extracted three times with ethyl acetate and the combined organic phases are washed with saturated aqueous sodium chloride solution, dried over sodium sulphate and concentrated. The residue is purified by preparative HPLC (with 0.1% TFA added).

1. stirringthe mixture is stirred at 60° C. overnight
2. extractionthe mixture is extracted three times with ethyl acetate
3. washthe combined organic phases are washed with saturated aqueous sodium chloride solution
4. dry with materialdried over sodium sulphate
5. concentrationconcentrated
6. customThe residue is purified by preparative HPLC (with 0.1% TFA added)