反应详情

To a solution of 4-tert-butyl-N-[4-chloro-2-(4-hydroxymethyl-pyrazol-1-yl)-phenyl]-benzenesulfonamide (synthesized according to general procedure LL, 31 mg, 0.074 mmol) in CH2Cl2 (3 mL) was added Dess-Martin periodinane (34 mg, 0.33 mmol) and the reaction was stirred for 3 hours at room temperature. 10% Na2S2O3 (5 mL) and saturated aqueous NaHCO3 (5 mL) were added sequentially and the mixture was stirred an additional 30 minutes. The aqueous layer was subsequently separated and extracted with EtOAc (2×25 mL). The combined organic layers were washed with saturated aqueous NaHCO3 solution (20 mL) and brine (20 mL), dried (anhydrous Na2SO4), and concentrated in vacuo to afford 4-tert-butyl-N-[4-chloro-2-(4-formyl-pyrazol-1-yl)-phenyl]-benzenesulfonamide which was used for further transformation without purification.

1. stirringthe mixture was stirred an additional 30 minutes
2. customThe aqueous layer was subsequently separated
3. extractionextracted with EtOAc (2×25 mL)
4. washThe combined organic layers were washed with saturated aqueous NaHCO3 solution (20 mL) and brine (20 mL)
5. dry with materialdried (anhydrous Na2SO4)
6. concentrationconcentrated in vacuo