反应详情

温度

0 °C

Under argon, 64 ml (0.81 mmol) of cyclobutyl alcohol were initially charged in dichloromethane (4.1 ml), 161 mg (0.54 mmol) of bis(trichloromethyl)carbonate were then added and the mixture was cooled to 0° C. 53 μl (0.65 mmol) of pyridine were then added dropwise, and the reaction mixture was stirred at 0° C. for another 30 min. 200 mg (0.54 mmol) of the compound from example 6A were then added, and the mixture was diluted with 1.4 ml of pyridine. The reaction mixture was stirred at RT overnight, saturated aqueous sodium bicarbonate solution was then added and the mixture was extracted twice with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue was purified by means of preparative RP-HPLC (acetonitrile:water (+0.1% formic acid)−gradient) and the product fractions were concentrated.

1. stirringThe reaction mixture was stirred at RT overnight
2. extractionthe mixture was extracted twice with ethyl acetate
3. dry with materialThe combined organic phases were dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated
6. customThe residue was purified by means of preparative RP-HPLC (acetonitrile:water (+0.1% formic acid)−gradient)
7. concentrationthe product fractions were concentrated