HRID36613
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
- 85 °C
PROCEDURE
实验过程
Zinc dust (1.3 g, 20 mmol) is added to a solution of the crude product from step A in 20 mL glacial acetic acid maintained at 85° C. The reaction mixture is filtered after 30 minutes and concentrated in vacuo. The residue is then diluted with water, basified with a 1.0N aqueous NaOH solution, and extracted with CH2Cl2. The extract is dried with Na2SO4, filtered and concentrated in vacuo. The residue is then purified via flash chromatography (MeOH/CH2Cl2) to provide the title compound.
WORKUP
后处理
- filtrationThe reaction mixture is filtered after 30 minutes
- concentrationconcentrated in vacuo
- additionThe residue is then diluted with water
- extractionextracted with CH2Cl2
- dry with materialThe extract is dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe residue is then purified via flash chromatography (MeOH/CH2Cl2)