反应详情

98 mg (0.1 mmol) of the compound from example 15A was dissolved in approx. 4 ml tetrahydrofuran. 70 μl (0.5 mmol) Triethylamine, 19 μl (0.5 mmol) formic acid and 11 mg (0.01 mmol) tetrakis(triphenylphosphin)palladium(0) were added. The reaction mixture was stirred over night at room temperature. The reaction was diluted with approx. 5 ml water and twice extracted with approx. 5 ml dichloromethane. The combined organic phases were extracted with brine, dried over sodium sulfate and concentrated to dryness under reduced pressure. The raw product was purified by preparative RP-HPLC on a C18 column with a water/methanol gradient to yield 67 mg (79% of theory) product.

1. extractiontwice extracted with approx. 5 ml dichloromethane
2. extractionThe combined organic phases were extracted with brine
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated to dryness under reduced pressure
5. customThe raw product was purified by preparative RP-HPLC on a C18 column with a water/methanol gradient
6. customto yield 67 mg (79% of theory) product