Réaction #2460328

ord-4160a45f63744d99a0b8e64e53335438

Équation de réaction

CCCCc1ccc(N2c3ccccc3Sc3ccccc32)cc1
10-(4-butylphenyl)-10H-phenothiazine
F[P-](F)(F)(F)(F)F.c1ccc([I+]c2ccccc2)cc1
diphenyliodonium hexafluorophosphate
CCCCc1ccc(N2c3ccccc3[S+](c3ccccc3)c3ccccc32)cc1.F[P-](F)(F)(F)(F)F
10-(4-butylphenyl)-5-phenyl-10H-phenothiazin-5-ium hexa-fluorophosphate

Solvants

Conditions de réaction

Température
120°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureUpon cooling to ambient temperature
  2. 2
    workup.ADDITIONwas added
  3. 3
    Lavagewashed with ether
  4. 4
    Filtrationcollected by filtration
  5. 5
    Lavagewashed three times with ether
  6. 6
    AutreWithout further purification
  7. 7
    Autreit was isolated in 98.2% (2.36 g)
  8. 8
    Autreyield as a pale yellow solid

Mode opératoire

A mixture of 10-(4-butylphenyl)-10H-phenothiazine (83) (1.44 g, 4.34 mmol), diphenyliodonium hexafluorophosphate (1.85 g, 4.34 mmol) and copper (I) benzoate (0.10 g) was heated at 120° C. for 3 hours under nitrogen. Upon cooling to ambient temperature, the mixture was transferred to a mortar-and-pestle and 50 ml of ether was added. The solid was finely powdered, washed with ether, collected by filtration and washed three times with ether. Without further purification, it was isolated in 98.2% (2.36 g) yield as a pale yellow solid.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US07459106B2uspto-grants-2008_12