反应详情

To a solution of 2b (272 mg, 1.00 mmol) in dry toluene (4.0 mL) was added Bredereck's reagent (183 mg, 1.05 mmol) dropwise over 2 minutes. The mixture stirred at rt for 1 h and heated to 60° C. for 24 h. The mixture was concentrated and the residue purified on a SiO2 column (CH2Cl2, 50% EtOAc-hexanes then EtOAc for elution) to give a viscous oil. The oil was dissolved in 50% Et2O-hexanes and concentrated to give the title compound 3b as a waxy white solid; 243 mg, 74%. This material was used immediately without further purification.

1. temperatureheated to 60° C. for 24 h
2. concentrationThe mixture was concentrated
3. customthe residue purified on a SiO2 column (CH2Cl2, 50% EtOAc-hexanes
4. washEtOAc for elution)
5. customto give a viscous oil
6. concentrationconcentrated