反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Di(1-naphthyl)sulfide (3 g, 0.0104 mole), diphenyliodonium triflate (5.8 g, 0.0135 mole) and copper benzoate (0.08 g, 0.003 mole) are heated without solvent for 3 hours at 120-145° C. under a nitrogen atmosphere. After cooling down, 75 ml ether was added and the mixture vigorously stirred overnight to achive solidification. Filtration and washing with ether yielded a brown solid, which was dissolved in hot water, the solution filtered and the water removed in vacuo. The resulting white solid was stirred in 50 ml ethyl ether for 24 hours, the mixture filtered and the residue washed with ethyl ether, yielding 4.8 g (90%) of the title compound, di-(1-naphthyl)phenylsulfonium triflate. The structure was confirmed by 1H/13C NMR spectroscopy.
WORKUP
后处理
- temperatureAfter cooling down
- customthe mixture vigorously stirred overnight
- filtrationFiltration
- washwashing with ether
- customyielded a brown solid, which
- filtrationthe solution filtered
- customthe water removed in vacuo
- filtrationthe mixture filtered
- washthe residue washed with ethyl ether