Reaktion #472263

Reaktionsgleichung

3-(3-chloro-4-methoxy-5-trifluoromethylbenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole

lithium chloride

hydrochloric acid

→

title compound

Ausbeute 91.0%

3-(3-chloro-4-hydroxy-5-trifluoromethylbenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole

Ausbeute 91.0%

Lösungsmittel

N,N-dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Extraktionthe mixture was extracted with ethyl acetate
2. 2
   WaschenThe organic layer was washed with 1N hydrochloric acid and saturated brine
3. 3
   Trocknendried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   Sonstigethe obtained residue was crystallized from diethylether

Vorschrift

3-(3-chloro-4-methoxy-5-trifluoromethylbenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole (74 mg) was dissolved in N,N-dimethylformamide (2 mL), lithium chloride (77 mg) was added to the solution, and then the mixture was stirred at 70° C. for 22 hours. To the reaction solution, 1N hydrochloric acid was added, and then the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid and saturated brine, and then dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was crystallized from diethylether to obtain the title compound (65 mg) as a colorless crystal.

Quelle