Reaktion #1005967

ord-13081a8ed97b41faba1cd5e397742ba7

Reaktionsgleichung

Fc1cc(C(F)(F)F)ccc1Br
4-bromo-3-fluorobenzotrifluoride
CCS
ethanethiol
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CN(C)C=O
DMF
CCSc1cc(C(F)(F)F)ccc1Br
4-bromo-3-ethylsulfanylbenzotrifluoride

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Extraktionthe mixture was extracted with t-butyl methyl ether
  2. 2
    WaschenThe organic layer was washed with water
  3. 3
    Trocknendried over anhydrous magnesium sulfate
  4. 4
    Einengenconcentrated under reduced pressure

Vorschrift

A mixture of 1.5 g of 4-bromo-3-fluorobenzotrifluoride, 0.46 ml of ethanethiol, 851 mg of potassium carbonate and 2 ml of DMF was stirred at 75° C. for 2.5 hours. Water was poured to the cooled reaction mixture, and the mixture was extracted with t-butyl methyl ether. The organic layer was washed with water, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 1.15 g of 4-bromo-3-ethylsulfanylbenzotrifluoride.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09271500B2uspto-grants-2016_03