تفاعل #1602570

ord-e6466d27c82a4b7082a4cf9bdcf330e7

معادلة التفاعل

CCCCC(=O)OCC(F)(F)S(=O)(=O)[O-].[Na+]
sodium 1,1-difluoro-2-(valeryloxy)ethanesulfonate
CCCCC(=O)OCC(F)(F)S(=O)(=O)[O-].[Na+]
sodium 2-valeryloxy-1,1-difluoroethane sulfonate
[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
CCCCC(=O)OCC(F)(F)S(=O)(=O)[O-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium 1,1-difluoro-2-(valeryloxy)ethanesulfonate
المردود 64.0%

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصThen, extraction
  2. 2
    workup.ADDITIONby adding 30 mL of chloroform
  3. 3
    غسيلThe obtained organic layer was rinsed two times with water
  4. 4
    workup.DISTILLATIONby distilling a solvent off,

الإجراء التجريبي

A 100 mL reactor was charged with 3.0 g (26% purity, 2.9 millimoles) of sodium 1,1-difluoro-2-(valeryloxy)ethanesulfonate obtained in Example 5-3 and 30 g of water, followed by adding dropwise an aqueous solution of triphenylsulfonium chloride [17.8 g (5.2 millimoles/1.8 equivalents) of triphenylsulfonium chloride and 16.2 g of water] at room temperature, followed by stirring at room temperature for 1.5 hours. Then, extraction was conducted by adding 30 mL of chloroform. The obtained organic layer was rinsed two times with water, followed by distilling a solvent off, thereby obtaining 0.96 g of the target triphenylsulfonium 1,1-difluoro-2-(valeryloxy)ethanesulfonate.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08222448B2uspto-grants-2012_07