Methyl triflate → 5,6-Dimethoxy-2,3-dimethylbenzotellurazolium Trifluoromethanesulfonate
反応式
[CH3:1][O:2][C:3]1[C:4]([O:13][CH3:14])=[CH:5][C:6]2[Te:10][C:9]([CH3:11])=[N:8][C:7]=2[CH:12]=1.[F:15][C:16]([F:23])([F:22])[S:17]([O:20]C)(=[O:19])=[O:18]>ClCCl>[F:15][C:16]([F:23])([F:22])[S:17]([O-:20])(=[O:19])=[O:18].[CH3:1][O:2][C:3]1[C:4]([O:13][CH3:14])=[CH:5][C:6]2[Te:10][C:9]([CH3:11])=[N+:8]([CH3:16])[C:7]=2[CH:12]=1参加物
4
実験手順
5,6-Dimethoxy-2-methylbenzotellurazole (Example 19) (4.8 g=0.013 mole) was dissolved in dichloromethane (75 ml), and methyl trifluoromethanesulfonate (2.48 g=1.66 ml=0.013 mole) was added. The solution turned cloudy and crystals started to deposit within a few minutes. Precipitation was completed by addition of diethyl ether. The product was collected by filtration to give 5.5 g, 86.5% of theory, m.p. 210°-234° C. The product was recrystallized from boiling acetone (≃130 ml required) m.p. 242°-243° C.