반응 #2446096
ord-204c9193d92d4364a927c2c4dc7ca029
반응 방정식
반응 조건
후처리
- 1기타equipped with a magnetic stirrer and a reflux condenser
- 2온도The mixture is refluxed
- 3온도The reaction mixture is heated to 60° C. internal temperature
- 4온도cooled down to room temperature
- 5추출The organic phase is extracted twice with water and once with brine
- 6건조The organic phase is dried over Sodiumsulfate
- 7기타the solvent evaporated
- 8기타The crude product is purified by column chromatography (Heptane)
실험 절차
16.09 g (0.259 mol) of Potassium hydroxide (86%) are placed in a 500 ml three necked round bottomed flask equipped with a magnetic stirrer and a reflux condenser. 200 ml of THF and 6.5 ml of Dichloromethane are added. The mixture is refluxed. After 1 hour the mixture is cooled to room temperature. A solution of 8 g (37.74 mmol) dibenzofuran-4-boronic acid, 0.8 g (3.02 mmol) of Triphenylphosphine, 339 mg (0.7 mmol) of Palladium (II) acetate and 200 ml of Methanol are added. The reaction mixture is heated to 60° C. internal temperature. After 2 hours the reaction is complete and cooled down to room temperature. The mixture is diluted with H2O and Ethylacetate. The organic phase is extracted twice with water and once with brine. The organic phase is dried over Sodiumsulfate and the solvent evaporated. The crude product is purified by column chromatography (Heptane). 4-Vinyl-dibenzofuran is isolated in 42% yield.