HRID1640098

反应详情

EQUATION

反应方程式

HRID 1640098 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 20% titanium trichloride (8.4 g) was added to a mixture of 4-(3,5-bis-trifluoromethyl-benzyl)-2-methyl-nitrobenzene (0.44 g), ammonium acetate (9.3 g), acetone (20 ml) and water (10 ml) at room temperature and stirred for 12 hours. After the reaction, the reaction solution was extracted with ethyl acetate and washed with a saturated sodium bicarbonate solution and a saturated salt solution and then dried over anhydrous magnesium sulfate. After distilling the solvent off, the resultant residue was purified by silica gel column chromatography to obtain 4-(3,5-bis-trifluoromethyl-benzyl)-2-methylaniline (0.22 g).

WORKUP

后处理

  1. customAfter the reaction
  2. extractionthe reaction solution was extracted with ethyl acetate
  3. washwashed with a saturated sodium bicarbonate solution
  4. dry with materiala saturated salt solution and then dried over anhydrous magnesium sulfate
  5. distillationAfter distilling the solvent off, the resultant residue
  6. customwas purified by silica gel column chromatography