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Imidazole → 4-(t-Butyldiphenylsilyloxy)-1-methyl-1-butanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Pentane-1,4-diol | HCID 79083 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-(t-Butyldiphenylsilyloxy)-1-methyl-1-butanol | HCID 23028571 | — |
反応手順
In N,N-dimethylformamide (200 ml) were dissolved 1,4-pentanediol (10.0 g, 96.0 mmol) and imidazole (6.6 g, 96.9 mmol). Under ice cooling, t-butyl chlorodiphenylsilane (25.2 ml, 96.4 mmol) was added dropwise. After completion of the dropwise addition, the reaction mixture was stirred at room temperature for 2 days. To the reaction mixture was added diethyl ether, followed by washing with water. The organic layer was dried over anhydrous magnesium sulfate. After filtration, the residue obtained by concentrating the filtrate under reduced pressure was purified by silica gel chromatography (hexane:ethyl acetate=5:1), whereby the title compound (32.0 g, 97%) was obtained as a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07399775B2 |
| 出典データセット | uspto-grants-2008_07 |
| ORD ID | ord-70b62e78ab69429c94b4d30757a4585a |
| 出典メモ | uspto-grants-2008_07 |