反应详情

温度

80 °C

18.7 cm3 (50 mmol) of a 20% strength solution of butyl-lithium in toluene were added at room temperature to a solution of 10 g (50 mmol) of 10 in 100 cm3 of H2O- and O2 -free toluene and 5 ml of H2O- and O2 -free THF, and the mixture was heated at 80° C. for 2 hours. The yellow suspension was subsequently cooled to 0° C., and 3.2 g (25 mmol) of dimethyldichlorosilane were added. The reaction mixture was heated at 80° C. for a further 1 hour and subsequently washed with 50 cm3 of H2O. The solvent was removed in vacuo, and the residue was recrystallized from heptane at -20° C., giving 6.7 g (62%) of 11 as colorless crystals (m.p. 109°-110° C.).

1. temperatureThe yellow suspension was subsequently cooled to 0° C.
2. temperatureThe reaction mixture was heated at 80° C. for a further 1 hour
3. washsubsequently washed with 50 cm3 of H2O
4. customThe solvent was removed in vacuo
5. customthe residue was recrystallized from heptane at -20° C.