Tetramethoxysilane → 2-(Trimethoxysilyl)thianthrene

反応式

[Mg].[CH3:2][O:3][Si:4](OC)([O:7][CH3:8])[O:5][CH3:6].Br[C:12]1[CH:25]=[CH:24][C:23]2[S:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[S:15][C:14]=2[CH:13]=1>C1COCC1>[CH3:2][O:3][Si:4]([O:7][CH3:8])([O:5][CH3:6])[C:12]1[CH:25]=[CH:24][C:23]2[S:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[S:15][C:14]=2[CH:13]=1

参加物

実験手順

A 3-neck 1 L flask was filled with magnesium turnings (5 g), THF (200 g) and tetramethoxysilane (50 g), and heated to reflux. 2-Bromothianthrene (40 g), prepared analogously to Example 3A was added to the flask in 10 g portions. Grignard started within 10 minutes. The reaction was allowed to cool for 1 hour, after which magnesium salts were precipitated with hexanes (200 mL). GC/MS of the solution showed that along with some thianthrene, 2-(trimethoxysilyl)thianthrene was obtained in ˜60% yield (FIG. 7).