تفاعل #1095841
ord-f5149a68d27c46f0882d718c622b61aa
معادلة التفاعل
الكواشف
ظروف التفاعل
المعالجة
- 1درجة الحرارةthe reaction solution was refluxed for 11.5 hours
- 2أخرىthe palladium powder was removed by cotton filtration
- 3أخرىThe product was purified by column chromatography (HexH:AcOEt=4:1)
الإجراء التجريبي
To a dioxane solution (10 mL) of triphenylphosphine (139 mg, 0.53 μmol), palladium acetate (40.0 mg, 0.18 μmol) and triethylamine (0.59 μL, 4.23 mmol) were sequentially added, and the mixture was stirred for 5 minutes at 75° C. A dioxane solution (15 mL) of compound 1 (1.03 g, 3.52 mmol) and acrylonitrile (0.46 μL, 7.04 mmol) were added, and the reaction solution was refluxed for 11.5 hours. The product was confirmed by TLC (HexH:AcOEt=4:1), and then the palladium powder was removed by cotton filtration. The product was purified by column chromatography (HexH:AcOEt=4:1), and compound 2 (0.14 g, 18%, trans:cis=97:3) was obtained as a white powder, while compound 1 (0.37 g, recovery rate 37%) was recovered as a white powder.