반응 #472329

반응 방정식

3-(3-cyano-4-methoxy-5-trifluoromethoxybenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole

lithium chloride

hydrochloric acid

→

title compound

수율 63.5%

3-(3-cyano-4-hydroxy-5-trifluoromethoxybenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole

수율 63.5%

용매

N,N-dimethylformamide

반응 조건

후처리

1. 1
   추출the mixture was extracted with ethyl acetate
2. 2
   세척The organic layer was washed with 1N hydrochloric acid and saturated brine
3. 3
   건조dried over anhydrous sodium sulfate
4. 4
   workup.DISTILLATIONThe solvent was distilled off under reduced pressure
5. 5
   기타the obtained residue was crystallized from n-hexane-ethyl acetate

실험 절차

3-(3-cyano-4-methoxy-5-trifluoromethoxybenzoyl)-1,1-dioxo-2,3-dihydro-1,3-benzothiazole (300 mg) was dissolved in N,N-dimethylformamide (4 mL), and lithium chloride (309 mg) was added to the solution, and then the mixture was stirred at 100° C. for 1 hour. 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 n-hexane-ethyl acetate to obtain the title compound (184 mg) as a colorless crystal.

출처