반응 #1596953

반응 방정식

bromodibenzofuran

Compound 16-1

bromodibenzofuran

pyrazole

salicylaldoxime

cesium carbonate

→

Compound 17-1

수율 78.0%

Pyrazolyldibenzofuran

수율 78.0%

용매

DMF

반응 조건

후처리

1. 1
   기타is reacted
2. 2
   온도under reflux
3. 3
   온도with heating for 6 hours
4. 4
   workup.DISTILLATIONDMF is distilled off from the resulting mixture
5. 5
   온도by heating under reduced pressure
6. 6
   workup.ADDITIONEthyl acetate is added to the residue
7. 7
   여과the mixture is filtered with Celite
8. 8
   workup.ADDITIONa 1M sodium hydroxide aqueous solution is added to the obtained liquid
9. 9
   추출Organic layers extracted from the obtained mixture with ethyl acetate
10. 10
    건조are dried with sodium sulfate
11. 11
    농축The organic layers are concentrated

실험 절차

Under nitrogen current, a mixture containing 12.35 g (50 mmol) of bromodibenzofuran (Compound 16-1), 5.11 g (75 mmol) of pyrazole, 358 mg (2.5 mmol) of cuprous oxide (I), 1.37 g (10 mmol) of salicylaldoxime, 32.6 g (100 mmol) of cesium carbonate, and 100 ml of DMF is reacted under reflux with heating for 6 hours. DMF is distilled off from the resulting mixture by heating under reduced pressure. Ethyl acetate is added to the residue and the mixture is filtered with Celite, and a 1M sodium hydroxide aqueous solution is added to the obtained liquid. Organic layers extracted from the obtained mixture with ethyl acetate are dried with sodium sulfate. The organic layers are concentrated and refined by silica gel column chromatography to obtain 9.12 g (39 mmol) of Compound 17-1.

출처