反応 #2460328

ord-4160a45f63744d99a0b8e64e53335438

反応方程式

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

溶媒

反応条件

温度
120°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度Upon cooling to ambient temperature
  2. 2
    workup.ADDITIONwas added
  3. 3
    洗浄washed with ether
  4. 4
    ろ過collected by filtration
  5. 5
    洗浄washed three times with ether
  6. 6
    その他Without further purification
  7. 7
    その他it was isolated in 98.2% (2.36 g)
  8. 8
    その他yield as a pale yellow solid

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07459106B2uspto-grants-2008_12