Reaktion #1005961

ord-3888f7a4df22403fadecfbef95e3f411

Reaktionsgleichung

CCS(=O)(=O)c1ccccc1-n1cc2ccc(C(F)(F)F)cc2n1
2-(2-ethylsulfonylphenyl)-6-trifluoromethyl-2H-indazole
O=C1CCC(=O)N1Cl
N-chlorosuccinimide
O=S([O-])([O-])=S.[Na+].[Na+]
sodium thiosulfate
CCS(=O)(=O)c1ccccc1-n1nc2cc(C(F)(F)F)ccc2c1Cl
3-chloro-2-(2-ethylsulfonylphenyl)-6-trifluoromethyl-2H-indazole
Ausbeute 100.8%

Lösungsmittel

Reaktionsbedingungen

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
  5. 5
    WaschenThe resulting residue was washed with n-hexane

Vorschrift

A mixture of 226 mg of 2-(2-ethylsulfonylphenyl)-6-trifluoromethyl-2H-indazole, 86 mg of N-chlorosuccinimide and 2 ml of DMF was stirred at room temperature for 10 hours. A 10% aqueous sodium thiosulfate solution was poured to the reaction mixture, and the mixture was extracted with t-butyl methyl ether. The organic layer was washed with water and dried over anhydrous magnesium sulfate, then concentrated under reduced pressure. The resulting residue was washed with n-hexane to obtain 250 mg of 3-chloro-2-(2-ethylsulfonylphenyl)-6-trifluoromethyl-2H-indazole (hereinafter, referred to as Compound of Present Invention 3).

Quelle

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