関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Pentane | HCID 8003 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Cyclohexane ethylacetate | HCID 21867204 | — |
| 生成物 | Silane, (4-bromophenoxy)(1,1-dimethylethyl)diphenyl- | HCID 11292808 | — |
反応手順
400 ml of dimethylformamide, 31.18 g of imidazole and 125.89 g of 1,1-dimethyl-ethyl-diphenyl-chlorosilane are added under an inert atmosphere and at ambient temperature to 80.89 g of parabromophenol, then the solution obtained is agitated for 2 hours. The reaction medium is poured into 2 liters of water, precipitation is observed, the solid is solubilized with ethyl acetate and the aqueous phase is extracted with ethyl acetate, the combined organic phases are dried and evaporated under reduced pressure until an oil is obtained. Pentane is added and crystallization is observed. After filtration and drying the precipitate 179.24 g of expected product is obtained. RF: 0.53 (thin layer chromatography, support: silica, eluant cyclohexane/AcOEt 95/5).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06365775B1 |
|---|
| 出典データセット | uspto-grants-2002_04 |
|---|
| ORD ID | ord-47d6756f54934686a60a341aebee27eb |
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| 出典メモ | uspto-grants-2002_04 |
|---|
