反应详情

温度

22 °C

A 0° C. solution of the product from step g) (874 mg, 4.05 mmol) in CH2Cl2 (20 ml) was treated with triethylamine (1.69 ml, 12.15 mmol) and ethyl chloroformate (466 μl, 4.86 mmol) and the reaction was warmed to 22° C. Next, the reaction mixture was diluted with CH2Cl2 (50 ml) and washed with brine (25 ml). The organic layer was dried (MgSO4) and solvent evaporated in vacuo leaving the crude product that was purified by silica-gel chromatography (hexanes:EtOAc-50:50) to give 722 mg (71%) of the subtitle compound. MS calculated for C13H17NO2S+H 252, observed 252.

1. washwashed with brine (25 ml)
2. dry with materialThe organic layer was dried (MgSO4) and solvent
3. customevaporated in vacuo
4. customleaving the crude product that
5. customwas purified by silica-gel chromatography (hexanes:EtOAc-50:50)