反应详情

温度

110 °C

At 60° C., 475.6 mg (3.12 mmol) of sodium chloro(difluoro)acetate were added to a mixture of 800.0 mg (1.73 mmol) of (+/−)-tert-butyl 1-(3-{[cyclopentyl(4-formylphenyl)acetyl]-amino}benzyl)cyclopropanecarboxylate and 681.9 mg (2.60 mmol) of triphenylphosphine. The mixture was heated to 110° C. and stirred at this temperature for 30 min. After cooling, the mixture was poured into water. Ethyl acetate was added, and the organic phase was separated off, washed with saturated sodium chloride solution, dried with magnesium sulphate and concentrated under reduced pressure. The crude product was purified by preparative RP-HPLC (mobile phase acetonitrile/water). This gave 319.2 mg (37.2% of theory) of the target compound.

1. temperatureAfter cooling
2. customthe organic phase was separated off
3. washwashed with saturated sodium chloride solution
4. dry with materialdried with magnesium sulphate
5. concentrationconcentrated under reduced pressure
6. customThe crude product was purified by preparative RP-HPLC (mobile phase acetonitrile/water)