HRID30282
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 22 °C
PROCEDURE
实验过程
A 0° C. solution of product from Example 29, step h) (885 mg, 4.1 mmol) in CH2Cl2 (20 ml) was treated with triethylamine (1.71 ml, 12.3 mmol) and ethyl chloroformate (472 μl, 4.92 mmol) and the reaction was warmed to 22° C. Next, the reaction mixture was diluted with CH2Cl2 (20 ml) and washed with brine (25 ml). The organic layer was dried (MgSO4) and the solvent evaporated in vacuo to give the crude product that was purified by silica-gel chromatography (hexanes:EtOAc-50:50) to give 748 mg (73%) of the subtitle compound. MS calculated for C13H17NO2S+H 252, observed 252.
WORKUP
后处理
- washwashed with brine (25 ml)
- dry with materialThe organic layer was dried (MgSO4)
- customthe solvent evaporated in vacuo
- customto give the crude product that
- customwas purified by silica-gel chromatography (hexanes:EtOAc-50:50)