HRID439529

反应详情

EQUATION

反应方程式

HRID 439529 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe solution was evaporated
  2. customto remove the ethanol
  3. additionThe residue was treated with 2N NaOH to pH=13
  4. extractionThe mixture was extracted by CHCl3 (3×10 mL)
  5. dry with materialThe extract was dried (MgSO4)
  6. customevaporated