反应详情

101 mg (0.16 mmol) of the compound from example 87A were dissolved in 10 ml of trifluoroacetic acid, 188 mg (1.62 mmol) of triethylsilane were added and the mixture was heated to reflux for 18 h. The reaction mixture was admixed with water and ethyl acetate, and neutralized with saturated aqueous sodium hydrogencarbonate solution. The organic phase was dried over sodium sulfate and concentrated on a rotary evaporator. The residue was dried under high vacuum, and purified by means of preparative HPLC (eluent: methanol/water with 0.1% trifluoroacetic acid, gradient 30:70→90:10). 53 mg of the title compound were obtained (69% of theory).

1. temperaturethe mixture was heated
2. temperatureto reflux for 18 h
3. dry with materialThe organic phase was dried over sodium sulfate
4. concentrationconcentrated on a rotary evaporator
5. customThe residue was dried under high vacuum
6. custompurified by means of preparative HPLC (eluent: methanol/water with 0.1% trifluoroacetic acid, gradient 30:70→90:10)