Reacción #1269823

ord-b95efa034a014d89b4fb61cbb2ccf486

Ecuación de reacción

C=C(C)C(=O)OC(CC)C(F)(F)C(=O)OCC(F)(F)S(=O)(=O)[O-].[Na+]
sodium 2-[3-(methacryloyloxy)-2,2-difluoro-n-pentanoyloxy]-1,1-difluoroethanesulfonate
O
water
[Cl-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium chloride
C=C(C)C(=O)OC(CC)C(F)(F)C(=O)OCC(F)(F)S(=O)(=O)[O-].c1ccc([S+](c2ccccc2)c2ccccc2)cc1
triphenylsulfonium 2-[3-(methacryloyloxy)-2,2-difluoro-n-pentanoyloxy]-1,1-difluoroethanesulfonate

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroInto a 100-mL reaction vessel
  2. 2
    Otrosubjected to separation
  3. 3
    LavadoThe thus-obtained organic phase was washed four times with 10 mL of water
  4. 4
    Concentraciónconcentrated under a reduced pressure

Procedimiento

Into a 100-mL reaction vessel were added 2.82 g (purity: 24%, 1.74 mmol) of sodium 2-[3-(methacryloyloxy)-2,2-difluoro-n-pentanoyloxy]-1,1-difluoroethanesulfonate obtained in Preparation Example 4-1, 9 mL of water and 9 mL of chloroform. Further, 2.10 g (7.05 mmol) of triphenylsulfonium chloride was dropped into the reaction vessel at room temperature. The resulting solution was stirred for 2 hours at room temperature and subjected to separation. The thus-obtained organic phase was washed four times with 10 mL of water and concentrated under a reduced pressure. With this, 3.00 g of target triphenylsulfonium 2-[3-(methacryloyloxy)-2,2-difluoro-n-pentanoyloxy]-1,1-difluoroethanesulfonate was obtained as a colorless oily substance. The purity of the target product was 53%; and the yield of the target product was 100%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08663897B2uspto-grants-2014_03