反応 #1596523

ord-57474eb564e549d09a43c60a3289c9c1

反応方程式

[Cl-].c1ccc([I+]c2ccccc2)cc1
diphenyliodonium chloride
CC(C)(C)C(=O)OCC(F)(F)S(=O)(=O)[O-].CC[NH+](CC)CC
triethylammonium 2-pivaloyloxy-1,1-difluoroethanesulfonate
O
water
CC(C)(C)C(=O)OCC(F)(F)S(=O)(=O)[O-].c1ccc([I+]c2ccccc2)cc1
target compound
収率 96.6%
CC(C)(C)C(=O)OCC(F)(F)S(=O)(=O)[O-].c1ccc([I+]c2ccccc2)cc1
Diphenyliodonium 2-Pivaloyloxy-1,1-difluoroethanesulfonate
収率 96.6%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他reacted at room temperature for 3 hours
  2. 2
    その他The thus-obtained reaction solution
  3. 3
    その他was separated into an organic layer
  4. 4
    洗浄The organic layer was washed five times with 15 mL of water
  5. 5
    濃縮subjected to concentration under reduced pressure

実験手順

In 10 mL of chloroform, 5 g of a solid of triethylammonium 2-pivaloyloxy-1,1-difluoroethanesulfonate (equivalent to 14.4 mmol) was dissolved by stirring. The resulting solution was admixed with 15 mL of water and 4.78 g (15.1 mmol) of diphenyliodonium chloride, and then, reacted at room temperature for 3 hours. The thus-obtained reaction solution was separated into an organic layer and an aqueous layer. The organic layer was washed five times with 15 mL of water and subjected to concentration under reduced pressure. With this, 7.32 g of the target compound was obtained as a white solid (purity: 90%, yield: 90%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09221928B2uspto-grants-2015_12