Reaktion #472281

ord-bb128d9bf5674a55a5370a8d5241e85e

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.DISTILLATIONAfter the solvent was distilled off under reduced pressure, water
  2. 2
    workup.ADDITIONwas added
  3. 3
    Extraktionthe mixture was extracted with ethyl acetate
  4. 4
    WaschenThe organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine
  5. 5
    Trocknendried over anhydrous sodium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure
  7. 7
    Sonstigethe obtained residue was used for the synthesis of (g)

Vorschrift

2,3-dihydro-1,3-benzothiazole synthesized from 2-aminobenzenethiol (346 mg) and 37% formalin (0.23 mL) in the same manner as in Example 1 was dissolved in chloroform (4 mL), and triethylamine (0.43 mL) and 4-methoxy-3-methylsulfanyl-5-trifluoromethylbenzoyl chloride were added to the solution, and then the mixture was stirred at room temperature for 1 hour. After the solvent was distilled off under reduced pressure, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, 1N sodium hydroxide and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was used for the synthesis of (g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08367843B2uspto-grants-2013_02