反应详情

温度

50 °C

A solution of triethyl-(5-iodpent-1-inyl)silane (5.02 g, 16.3 mmol) and triphenylphosphine (3.94 g, 15 mmol) in absolute ethanol (100 mL) was stirred 4 h with reflux and overnight at 50° C. and then heated once again with reflux for 7 h. The reaction solution was then concentrated to low volume in a vacuum, the yellowish crystals formed were mixed with diethyl ether (50 mL) and stirred. The diethyl ether was itself concentrated to low volume in a vacuum and the crystals mixed with ethyl acetate (50 mL). After standing in the refrigerator for 24 h the crystals were aspirated, washed with cold ethyl acetate (50 mL) and dried in an exsiccator over phosphorus pentoxide.

1. temperatureheated once again
2. temperaturewith reflux for 7 h
3. concentrationThe reaction solution was then concentrated to low volume in a vacuum
4. customthe yellowish crystals formed
5. concentrationconcentrated to low volume in a vacuum
6. additionthe crystals mixed with ethyl acetate (50 mL)
7. washwashed with cold ethyl acetate (50 mL)
8. dry with materialdried in an exsiccator over phosphorus pentoxide