Réaction #56612

ord-94a7ac36b8a0497681810865690b64ae

Équation de réaction

C[Si](C)(C)Cl
trimethylsilyl chloride
O=C(O)CCC(=O)c1ccc(-c2ccc(OC(F)(F)F)cc2)cc1
4-oxo-4-[4′-(trifluoromethoxy)-1,1′-biphenyl-4-yl]butyric acid
COC(C)(C)OC
2,2-dimethoxypropane
COC(=O)CCC(=O)c1ccc(-c2ccc(OC(F)(F)F)cc2)cc1
Methyl-4-oxo-4-[4′-(trifluoromethoxy)-1,1′-biphenyl-4-yl]butanoate

Solvants

Conditions de réaction

Température
50°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    ConcentrationThe reaction mixture is then concentrated
  2. 2
    Autrethe residue is recrystallized from toluene

Mode opératoire

Crude 4-oxo-4-[4′-(trifluoromethoxy)-1,1′-biphenyl-4-yl]butyric acid (25 g, content: 65%, GC, silylated, 100% method) is dissolved in a mixture of methanol (50 ml) and 2,2-dimethoxypropane (11.5 g, 110 mmol), treated with trimethylsilyl chloride (0.75 g, 7 mmol) and stirred at 50° C. for 16 h. The reaction mixture is then concentrated and the residue is recrystallized from toluene.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07419936B2uspto-grants-2008_09