反应详情

A solution of the product from step b) (863 mg, 2.62 mmol) in dioxane (13.1 ml) was treated with Pd(dppf)2Cl2 (128 mg, 0.157 mmol) and a 2M solution of dimethylzinc in toluene (2.62 ml, 5.24 mmol) at 102° C. for 1 h. The reaction was cooled to 220C and carefully quenched with sat. NH4Cl (3 ml). After the effervescence subsided, the reaction was extracted with EtOAc (3×50 ml). The combined organic extracts were dried (MgSO4), concentrated and eluted through a plug of silica-gel using 50:50 hexanes:EtOAc to give 411 mg (59%) of the subtitle compound. MS calculated for C14H19NO2S+H 266, observed 266.

1. customcarefully quenched with sat. NH4Cl (3 ml)
2. extractionthe reaction was extracted with EtOAc (3×50 ml)
3. dry with materialThe combined organic extracts were dried (MgSO4)
4. concentrationconcentrated
5. washeluted through a plug of silica-gel