反应详情

温度

100 °C

40 mg (0.12 mmol) of the compound from example 52A were initially charged in pyridine (5.0 ml), then 39 mg (0.13 mmol) of bis(trichloromethyl) carbonate were added and the mixture was stirred at 100° C. for 1 h. The reaction mixture was concentrated, admixed with saturated aqueous sodium hydrogencarbonate solution and extracted twice with ethyl acetate. The collected organic phases were dried over sodium sulfate, filtered and concentrated by rotary evaporation. The residue was separated by means of preparative HPLC (eluent: acetonitrile-water with 0.1% formic acid gradient) and the product fractions were concentrated. This gave 9 mg (20% of theory) of the title compound in solid form.

1. concentrationThe reaction mixture was concentrated
2. extractionextracted twice with ethyl acetate
3. dry with materialThe collected organic phases were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated by rotary evaporation
6. customThe residue was separated by means of preparative HPLC (eluent: acetonitrile-water with 0.1% formic acid gradient)
7. concentrationthe product fractions were concentrated