반응 #157997

반응 방정식

pyridine

4-amino-3-bromo-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]benzamide

4,5-dichloro-1,2,3-dithiazol-1-ium chloride

→

3-bromo-4-{[4-chloro-5H-1,2,3-dithiazol-5-ylidene]amino}-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]benzamide

수율 85.3%

용매

dichloromethane

tetrahydrofuran

반응 조건

후처리

1. 1
   workup.STIRRINGstirred at room temperature for 1 hour
2. 2
   기타The solvent was removed under reduced pressure
3. 3
   workup.ADDITIONTo the residue was added water
4. 4
   추출extracted twice with ethyl acetate
5. 5
   세척washed with water
6. 6
   건조dried over anhydrous magnesium sulfate
7. 7
   기타The drying agent (anhydrous magnesium sulfate) was removed by filtration
8. 8
   workup.DISTILLATIONthe solvent was distilled off under the reduced pressure
9. 9
   기타The residue was purified by column chromatography

실험 절차

4-amino-3-bromo-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]benzamide (0.254 g) was dissolved in tetrahydrofuran (20 ml). To the mixture was added 4,5-dichloro-1,2,3-dithiazol-1-ium chloride (0.106 g), and stirred at room temperature for 2 hours. To the reaction mixture was added pyridine (0.091 g) in dichloromethane, and stirred at room temperature for 1 hour. The solvent was removed under reduced pressure. To the residue was added water and extracted twice with ethyl acetate. The organic phases were combined and washed with water, and dried over anhydrous magnesium sulfate. The drying agent (anhydrous magnesium sulfate) was removed by filtration and the solvent was distilled off under the reduced pressure. The residue was purified by column chromatography to obtain 3-bromo-4-{[4-chloro-5H-1,2,3-dithiazol-5-ylidene]amino}-N-[2-ethyl-6-methyl-4-(1,1,1,2,3,3,4,4,4-nonafluorobutan-2-yl)phenyl]benzamide (0.270 g, 85%).

출처