反应详情

Reduction of 1,2-bis(o-anisylphenylphosphinyl) ethane was accomplished by refluxing 16.5 g. (0.12 mole) trichlorosilane and 12.2 g. (0.12 mole) triethylamine in 188 ml. of dry benzene for one hour. Then 3.0 g. (0.012 mole) of 1,2-bis(o-anisylphenylphosphinyl) ethane in 75 ml. of dry acetonitrile was added and the mixture refluxed 1.5 hours. Quenching in 30% sodium hydroxide solution followed by separating and evaporating the organic layer gave 1.4 g. of crude crystals which were insoluble in cold methanol. Further crystallization from hot methanol gave 1,2-bis(o-anisylphenylphosphino) ethane, m.p. 102°-104° C., [α]D20 -83.4° (C=0.5 in CHCl3). The mass spectra gave a very strong parent peak at 458 and the nmr confirmed the structure.

1. temperatureby refluxing 16.5 g
2. temperaturethe mixture refluxed 1.5 hours
3. customQuenching in 30% sodium hydroxide solution
4. customby separating
5. customevaporating the organic layer
6. customgave 1.4 g
7. customFurther crystallization from hot methanol