関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | Dichlorodimethylsilane | HCID 6398 | — |
| 反応物 | 1,2,3,4-Tetramethylcyclopentadiene | HCID 138163 | — |
| 反応物 | Butyllithium | HCID 178418339 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Chlorodimethyl(2,3,4,5-tetramethyl-2,4-cyclopentadien-1-yl)silane | HCID 5045335 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05521265 |
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| 出典データセット | uspto-grants-1996_05 |
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| ORD ID | ord-3c41bf2a3b2b46acbfa13f50f7c84a6a |
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| 出典メモ | uspto-grants-1996_05 |
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