HRID439529
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 solution of 122 mg (0.445 mmol) of 4,5-bis(trifluoromethyl)-2-nitroaniline and 498 mg (2.62 mmol) of SnCl2 in 6 mL of ethanol was heated at 70° C. for 2 h. The solution was evaporated to remove the ethanol. The residue was treated with 2N NaOH to pH=13. White precipitate was observed. The mixture was extracted by CHCl3 (3×10 mL). The extract was dried (MgSO4) and evaporated to leave 102 mg (94%) of oil. 1H NMR (CDCl3), 3.70 (mb, 4), 7.069 (s, 2) and some impurity. 19F NMR (CDCl3), 56.659 (s).
WORKUP
后处理
- customThe solution was evaporated
- customto remove the ethanol
- additionThe residue was treated with 2N NaOH to pH=13
- extractionThe mixture was extracted by CHCl3 (3×10 mL)
- dry with materialThe extract was dried (MgSO4)
- customevaporated