反应详情

4.0 g (32.8 mmol) of 1,2,3,4-tetramethylcyclopentadiene (F. X. Kohl; P. Jutzi, J. Organomet. Chem. 243 (1983) 119-121; G. Schmitt, S. Ozman, Chemikerzeitung 100 (1976), 143; E. E. Bunel; P. Campos, J. Ruz; L. Valle, Organometallics 7 (1988), 1828-1838; C. M. Fendrick; L. D. Schertz; V. W. Day; T. J. Marks, Organometallics 7, (1988) 1828-1838 and literature cited therein) are dissolved in 50 ml of absolute THF and admixed with 21 ml of n-butyllithium (1.6M in pentane, 33.6 mmol). The mixture is stirred for 2 hours and 4.50 g (33.3 mmol) of dimethyldichlorosilane, dissolved in 30 ml of absolute THF, are then added dropwise at 0° C. The mixture is subsequently stirred for a further 20 hours. After removal of the solvent in vacuo and filtering off the lithium chloride formed during the reaction, the residue is vacuum distilled. Bp: 57°-65° C. (P=0.1 torr).

1. additionare then added dropwise at 0° C
2. stirringThe mixture is subsequently stirred for a further 20 hours
3. customAfter removal of the solvent in vacuo
4. filtrationfiltering off the lithium chloride
5. customformed during the reaction
6. distillationdistilled