HRID227721
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
The product of Step (a) (10.0 g, 41.3 mmol, 1.00 equiv) was suspended in EtOH (120 mL). SnCl2.H2O (46.6 g, 206 mmol, 5.00 equiv) was added and the mixture was refluxed for 18 hours. The reaction mixture was concentrated en vacuo and water was added to the residue. The mixture was basified to pH 8 with satd. NaHCO3 and extracted with EtOAc (3×). The combined organic extracts were washed with satd. NaCl, dried over MgSO4, filtered and concentrated en vacuo. 8.10 g (92%) of the title compound was iolated as a purple solid.
WORKUP
后处理
- temperaturethe mixture was refluxed for 18 hours
- concentrationThe reaction mixture was concentrated en vacuo and water
- additionwas added to the residue
- extractionNaHCO3 and extracted with EtOAc (3×)
- washThe combined organic extracts were washed with satd
- dry with materialNaCl, dried over MgSO4
- filtrationfiltered
- concentrationconcentrated en vacuo