HRID1642630
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
PROCEDURE
实验过程
2-(3-Benzyloxy-4-nitrophenyl)-malonic acid tert-butyl ester ethyl ester (5.00 g, 12.0 mmol) is suspended in formic acid (60 mL) and stirred at RT for 18 h. The solvent is removed under reduced pressure and the residue taken up in EtOAc (100 mL). The organic solution is extracted with saturated NaHCO3 (2×50 mL) and brine (30 mL), before being dried over Na2SO4 and concentrated to an oil. Purification by flash column (10-15% EtOAc/hexanes) affords (3-benzyloxy-4-nitrophenyl)-acetic acid ethyl ester as a yellow oil: MS (M+H)+=316.
WORKUP
后处理
- customThe solvent is removed under reduced pressure
- extractionThe organic solution is extracted with saturated NaHCO3 (2×50 mL) and brine (30 mL)
- dry with materialbefore being dried over Na2SO4
- concentrationconcentrated to an oil
- customPurification by flash column (10-15% EtOAc/hexanes)