تفاعل #1596953
ord-70088dc7e64e46b5b9ca0cd3fc0d6742
معادلة التفاعل
المتفاعلات
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1أخرىis reacted
- 2درجة الحرارةunder reflux
- 3درجة الحرارةwith heating for 6 hours
- 4workup.DISTILLATIONDMF is distilled off from the resulting mixture
- 5درجة الحرارةby heating under reduced pressure
- 6workup.ADDITIONEthyl acetate is added to the residue
- 7ترشيحthe mixture is filtered with Celite
- 8workup.ADDITIONa 1M sodium hydroxide aqueous solution is added to the obtained liquid
- 9استخلاصOrganic layers extracted from the obtained mixture with ethyl acetate
- 10تجفيفare dried with sodium sulfate
- 11تركيزThe organic layers are concentrated
الإجراء التجريبي
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.