تفاعل #1596523

ord-57474eb564e549d09a43c60a3289c9c1

معادلة التفاعل

[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
المردود 96.6%
CC(C)(C)C(=O)OCC(F)(F)S(=O)(=O)[O-].c1ccc([I+]c2ccccc2)cc1
Diphenyliodonium 2-Pivaloyloxy-1,1-difluoroethanesulfonate
المردود 96.6%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىreacted at room temperature for 3 hours
  2. 2
    أخرىThe thus-obtained reaction solution
  3. 3
    أخرىwas separated into an organic layer
  4. 4
    غسيلThe organic layer was washed five times with 15 mL of water
  5. 5
    تركيزsubjected to concentration under reduced pressure

الإجراء التجريبي

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%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09221928B2uspto-grants-2015_12