HRID229730

反应详情

EQUATION

反应方程式

HRID 229730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a toluene solution (423 mL) of commercially available 3′-trifluoromethylacetophenone (79.6 g, 0.423 mol) was added pyridinium bromide perbromide (135.4 g, 0.423 mol) under ice cooling and stirred for 5 hours while heating up to room temperature. The reaction liquid was ice cooled again, followed by dropwise adding 400 mL of distilled water to stop reaction and fractionation. A toluene layer was washed with 400 mL of a saturated aqueous solution of sodium bicarbonate, followed by drying with magnesium sulfate anhydride and concentration under reduced pressure and distillation under reduced pressure to obtain an objective compound (92.35 g, 81.7%).

WORKUP

后处理

  1. customThe reaction liquid
  2. temperaturecooled again
  3. customreaction and fractionation
  4. washA toluene layer was washed with 400 mL of a saturated aqueous solution of sodium bicarbonate
  5. dry with materialby drying with magnesium sulfate anhydride and concentration under reduced pressure and distillation under reduced pressure