反应详情

温度

60 °C

(R)-4-((R)-1-(6-(1-tert-butyl-1H-pyrazol-4-yl)-3-(difluoromethyl)-3H-imidazo[4,5-c]pyridin-4-yloxy)ethyl)-1-((R)-1-(4-methoxyphenyl)ethyl)pyrrolidin-2-one 2.34 (max. 0.107 mmol) was dissolved in TFA (2 mL) and heated to 60° C. with stirring. After 15 h, the red solution was concentrated in vacuo and diluted with EtOAc (20 mL) and 1:1 saturated aqueous NaHCO3: brine (20 mL). The phases were separated and the aqueous phase was extracted with EtOAc (20 mL). The combined organic phase was dried over Na2SO4, filtered, and concentrated onto silica gel. Purification by silica gel chromatography (40% to 100% acetone in hexanes) provided (R)-4-((R)-1-(6-(1-tert-butyl-1H-pyrazol-4-yl)-3-(difluoromethyl)-3H-imidazo[4,5-c]pyridin-4-yloxy)ethyl)pyrrolidin-2-one 3.03.

1. concentrationthe red solution was concentrated in vacuo
2. additiondiluted with EtOAc (20 mL) and 1:1 saturated aqueous NaHCO3
3. customThe phases were separated
4. extractionthe aqueous phase was extracted with EtOAc (20 mL)
5. dry with materialThe combined organic phase was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated onto silica gel
8. customPurification by silica gel chromatography (40% to 100% acetone in hexanes)