반응 #84884

반응 방정식

tin(II) chloride dihydrate

3-(4-nitrophenyl)-1,2,4-oxadiazol-5(4H)-one

sodium bicarbonate

→

3-(4-Aminophenyl)-1,2,4-oxadiazol-5(4H)-one

용매

ethanol

반응 조건

후처리

1. 1
   workup.ADDITIONwas added carefully until a pH of 8
2. 2
   여과The mixture was filtered through a filter layer
3. 3
   세척the residue was washed with ethyl acetate
4. 4
   농축The combined filtrates were concentrated under reduced pressure
5. 5
   workup.STIRRINGThe residue was stirred with dichloromethane and methanol
6. 6
   workup.ADDITIONtreated in an ultrasonic bath for 10 min
7. 7
   여과filtered
8. 8
   농축The filtrate was concentrated under reduced pressure
9. 9
   기타dried

실험 절차

6.5 g (29 mmol, 4 eq.) of tin(II) chloride dihydrate were added to a solution of 1.5 g (7.2 mmol) of 3-(4-nitrophenyl)-1,2,4-oxadiazol-5(4H)-one in 75 ml of ethanol, and the mixture was stirred at 70° C. for 1 h. The reaction mixture was poured into ice-water, and sodium bicarbonate was added carefully until a pH of 8 had been reached. The mixture was filtered through a filter layer and the residue was washed with ethyl acetate. The combined filtrates were concentrated under reduced pressure. The residue was stirred with dichloromethane and methanol, treated in an ultrasonic bath for 10 min and then filtered. The filtrate was concentrated under reduced pressure and dried. Yield: 1.4 g (quant.)

출처