反应详情

To a solution of phenol (0.11 g, 1.16 mmol) in THF (5 mL) is added NaH (0.024 g of a 60% dispersion in mineral oil, 0.58 mmol). After stirring for 5 min at room temp, a solution of 4-[4-(4-fluorophenyl)-2-methyl-5-(2-methanesulfonyl-pyrimidin-4-yl)-3-oxo-2,3-dihydro-pyrazol-1-yl]-piperidine-1 carboxylic acid tert-butyl ester, 12, (0.154 g, 0.29 mmol) in THF (3 mL) is added all at once. The reaction mixture is stirred at room temp for 14 hours and then quenched by pouring into aqueous saturated NaHCO3 solution. The aqueous phase is extracted three times with CH2Cl2, the combined organic phases washed with saturated sodium bicarbonate, dried (MgSO4), filtered and concentrated in vacuo. The crude residue was used without further purification in the next step.

1. stirringThe reaction mixture is stirred at room temp for 14 hours
2. customquenched
3. additionby pouring into aqueous saturated NaHCO3 solution
4. extractionThe aqueous phase is extracted three times with CH2Cl2
5. washthe combined organic phases washed with saturated sodium bicarbonate
6. dry with materialdried (MgSO4)
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customThe crude residue was used without further purification in the next step