関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | Chlorotrimethylsilane | HCID 6397 | — |
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | 1-Iodo-3-methyloct-1-en-3-ol | HCID 54522683 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Iodo-3-methyl-3-trimethylsilyloxy-1-octene | HCID 54370316 | 99% |
反応手順
To a stirred solution of 11.7 g of 3-hydroxy-1-iodo-3-methyl-1-octene (Example 184) and 7.4 g of imidazole in 45 ml of dry dimethylformamide is added dropwise 5.98 g of trimethylsilylchloride at 0° C. under argon atmosphere. After stirring at 0° C. for an additional 15 minutes, the solution is stirred at ambient temperature for 18 hours. The reaction mixture is poured into 600 ml of hexane and the resulting solution washed with water, saturated sodium chloride solution, dried over anhydrous magnesium sulfate and taken to dryness to furnish 14.7 g of oil. Distillation affords 13.4 g of clear oil; bp 65° C. (0.05 mm); λ max 6.21, 8.00, 9.90, 10.51, 11.90, 13.2μ.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04235797 |
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| 出典データセット | uspto-grants-1980_11 |
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| ORD ID | ord-1332913e923c4111b16b38886940cfdc |
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| 出典メモ | uspto-grants-1980_11 |
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