HRID1258748
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
A mixture of N-(3-nitro-4-trifluoromethoxy-benzyl)-2,2-dimethyl-propionamide (3.4 g, 11 mmol), Fe (3.7 g, 66 mmol), saturated aqueous NH4Cl-solution (35 mL) and EtOH (170 mL) was refluxed for 30 min. The mixture was concentrated, treated with water and the pH was adjusted to ˜8. The mixture was extracted with EtOAc and the organic layer was dried over Na2SO4, filtered and concentrated. The residue was treated with PE and the sub-title compound was filtered off. Yield: 2.7 g (88%).
WORKUP
后处理
- temperaturewas refluxed for 30 min
- concentrationThe mixture was concentrated
- additiontreated with water
- extractionThe mixture was extracted with EtOAc
- dry with materialthe organic layer was dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- additionThe residue was treated with PE
- filtrationthe sub-title compound was filtered off