反应详情

1-Bromopyrene (10 mmol), C6H5NH2 (12 mmol), Pd(dba)2 (0.20 mmol), P(t-Bu)3 (0.20-0.30 mmol) and sodium t-butoxide (1.44 g, 15 mmol) were charged in a two-necked flask under a nitrogen atmosphere. Toluene (25 ml) was added and the resulting violet solution was stirred at room temperature for 8 hours. During this period the contents of the flask became a pale yellow fluorescent solution. The reaction was quenched with water (30 ml) and the organic layer was taken into 100 ml diethyl ether, washed with brine solution, and dried over MgSO4. Evaporation of the solvent under vacuum resulted in a yellow solid that was adsorbed in silica gel and purified by column chromatography using dichloromethane/hexane (1:1) as eluant to produce phenyl-pyren-1-yl-amine (89%).

1. waitDuring this period the contents of the flask became
2. customThe reaction was quenched with water (30 ml)
3. washwashed with brine solution
4. dry with materialdried over MgSO4
5. customEvaporation of the solvent under vacuum
6. customresulted in a yellow solid
7. custompurified by column chromatography