反应详情

温度

22 °C

A solution of the product from step j) (284 mg, 0.86 mmol) in dioxane (4.3 ml) was treated with Pd(dppf)2Cl2 (42 mg, 0.051 mmol) and a 2M solution of dimethylzinc in toluene (0.86 ml, 1.72 mmol) at 102° C. for 1 hour. The reaction was cooled to 22° C. and carefully quenched with sat. NH4Cl (3 ml). After the effervescence subsided, the reaction was extracted with EtOAc (3×50 ml). The combined organic layers were dried (MgSO4) passed through a plug of silica-gel eluting with 50:50 hexanes:EtOAc to provide the subtitle compound (216 mg, 95% over 3-steps). 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 layers were dried (MgSO4)
4. washeluting with 50:50 hexanes