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Imidazole → 7-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne
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 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | 7-Chloro-4-hydroxy-4-methyl-1-heptyne | HCID 12898739 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 7-Chloro-4-methyl-4-trimethylsilyloxy-1-heptyne | HCID 12898740 | — |
反応手順
To a solution of 7-chloro-4-hydroxy-4-methyl-1-heptyne in 80 ml. of dimethylformamide at 0° C., is added 43.8 g. (0.644 moles) of imidazole and 35.02 g. (0.322 moles of) chlorotrimethylsilane. The mixture is stirred at room temperature for 45 minutes, poured into water and extracted with hexane. The hexane solution is washed with dilute sodium bicarbonate solution, dried over magnesium sulfate and the solvent removed leaving an orange liquid. This liquid is distilled giving the desired product in the fraction boiling at 83°-88° C., 1.5 mm. as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04297516 |
| 出典データセット | uspto-grants-1981_10 |
| ORD ID | ord-b7c5028134d745a0a0fa14369ca28170 |
| 出典メモ | uspto-grants-1981_10 |