HRID2217783

反应详情

EQUATION

反应方程式

HRID 2217783 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 100 mL of a tetrahydrofuran solution of 24.00 g (100 mmol) of 4-benzyloxypropiophenone, a hexane solution (20 mL) of 23.973 g (1.5 equivalents) of bromine was gradually added at 20° C., followed by 1 hour of stirring. To the resulting solution, 50 mL of a saturated sodium hydrogen carbonate solution and 100 mL of ethyl acetate were added to conduct extraction. The organic layer was washed with 30 mL of a 20 wt % sodium thiosulfate aqueous solution, dried over anhydrous magnesium sulfate, and subjected to distillation under a reduced pressure to remove the solvents. A colorless, oily substance was obtained as a result. To this substance, 200 mL of hexane was added to precipitate crystals. White crystals (31.12 g; isolation yield: 95%) of 1-[4-(benzyloxy)phenyl]-2-bromo-1-propanone were obtained as a result.

WORKUP

后处理

  1. extractionextraction
  2. washThe organic layer was washed with 30 mL of a 20 wt % sodium thiosulfate aqueous solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationsubjected to distillation under a reduced pressure
  5. customto remove the solvents
  6. customA colorless, oily substance was obtained as a result
  7. customto precipitate crystals