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Imidazole → (3,5-Dichlorophenoxy)tris(propan-2-YL)silane
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 | 3,5-Dichlorophenol | HCID 11571 | — |
| 反応物 | Triisopropylsilyl chloride | HCID 139400 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (3,5-Dichlorophenoxy)tris(propan-2-YL)silane | HCID 21594466 | 97.4% |
反応手順
To a mixture of 3,5-dichlorophenol (16.3 g, 100 mmol), imidazole (14.98 g, 220 mmol), and triisopropylchlorosilane (21.21 g, 110 mmol) was added DMF (200 mL) at room temperature. The resulting brown solution was stirred for 15 h and then it was diluted with water (500 mL). The organic compound was extracted into ethyl acetate (2×100 mL) and the combined organic layer was washed with brine solution and dried over anhydrous MgSO4. Filtration and concentration gave the crude residue which was purified using an ISCO (400 g) column chromatography to obtain 31.1 g (97%) of (3,5-dichlorophenoxy)-triisopropylsilane as a colorless oil. EI(+)-HRMS m/e calcd. for C15H24Cl2OSi (M)+ 318.0973, obsd. 318.0971.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447035B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-a17d2cdcd2c949aab7f4b4f023a6eabf |
| 出典メモ | uspto-grants-2016_09 |