Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Trimethyltin chloride | HCID 14016 | — |
| Edukt | Ammonium Chloride | HCID 25517 | — |
| Edukt | HCID 178418370 | HCID 178418370 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | Stannane, trimethyl(4-methylphenyl)- | HCID 617834 | — |
Reaktionsschritte
p-Tolylmagnesium bromide solution (Aldrich) (1.0M solution in diethyl ether) (53 ml, 0.0530 mol) was added dropwise to trimethyltin chloride (6.92 g, 0.0347 mol) in tetrahydrofuran (50 ml) under nitrogen at -10° C. The suspension was allowed to warm slowly to room temperature over 3 h then saturated ammonium chloride solution (10 ml) was added followed by sufficient water to dissolve the precipitate. The solution was extracted three times with diethyl ether-hexane (1:1). The combined organic phase was washed with brine, dried (magnesium sulfate) and the solvents removed in vacuo. Vacuum distillation of the residue afforded a colorless liquid (39°-40 ° C., 0.1 mm Hg) which was further purified by flash chromatography (silica gel, hexane) to give p-tolyltrimethyltin as a colorless liquid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US05412097 |
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| Quelldatensatz | uspto-grants-1995_05 |
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| ORD ID | ord-83450f01458d44f9ba9916ff859c6a4a |
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| Quellennotiz | uspto-grants-1995_05 |
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