反应详情

In a dry box, a 1 liter three-necked, round-bottomed flask equipped with a stir-bar, a dropping funnel and a reflux condenser was charged with 75.0 g (3.26 mol) of sodium metal. The flask was attached to a Schlenk manifold, evacuated and flushed with nitrogen. THF (70 ml) and hexane (420 ml) were added and the dropping funnel was charged with 150 ml (1.44 mol) of methyldichlorosilane. Methyldichlorosilane was added slowly into the flask over a 3 hour period. The reaction solution turned purple and by the end of the addition was at gentle reflux. The reaction mixture was stirred at room temperature for 2 hours and then heated at reflux for 16 hours. After it had been cooled to room temperature, the reaction mixture (except for the large NaCl crystals) was transferred via cannula into a heavy-walled glass bottle. The mixture was centrifuged and the clear, colorless supernatant layer transferred by cannula into a 1 liter round-bottomed flask equipped with a stir-bar. Hexane (200 ml) and THF (20 ml) were added to the remaining solids, the mixture again was centrifuged, and the supernatant liquid combined with the supernatant solution previously separated. Solvent was removed by trap-to-trap distillation until the volume of the residue was about 100 ml, and the remaining liquid was transferred by cannula into a weighed 250 ml round-bottomed flask. Remaining solvent was removed by trap-to-trap distillation at approximately 0.05 mm Hg at room temperature to give 51.2 g (81%, 1.16 mol) of a cloudy white oil.

1. customIn a dry box, a 1 liter three-necked, round-bottomed flask equipped with a stir-bar, a dropping funnel and a reflux condenser
2. customThe flask was attached to a Schlenk
3. custommanifold, evacuated
4. customflushed with nitrogen
5. additionTHF (70 ml) and hexane (420 ml) were added
6. additionThe reaction solution turned purple and by the end of the addition
7. temperatureheated
8. temperatureat reflux for 16 hours
9. temperatureAfter it had been cooled to room temperature
10. customthe clear, colorless supernatant layer transferred by cannula into a 1 liter round-bottomed flask
11. customequipped with a stir-bar
12. custompreviously separated
13. customSolvent was removed by trap-to-trap
14. distillationdistillation until the volume of the residue
15. customthe remaining liquid was transferred by cannula into a weighed 250 ml round-bottomed flask
16. customRemaining solvent was removed by trap-to-trap
17. distillationdistillation at approximately 0.05 mm Hg at room temperature