関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-Iodobenzonitrile | HCID 76467 | — |
| 反応物 | 2-Octanol, 1,1,1-trifluoro- | HCID 97804 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | p-(1-Trifluoromethyl-heptyloxy)-benzonitrile | HCID 15724839 | — |
反応手順
Into 100 ml of dry DMF containing 0.86 g of sodium hydride (purity 60%), were added dropwise 3.9 g of R-form oa 1-trifluoromethyl-heptanol, at room temperature with such a speed not causing too rapid generation of hydrogen, to prepare sodium salt (alkoxide) of R-form oa 1-trifluoromethyl-heptanol. After addition was over, stirring was continued further an hour at room temperature, followed by adding thereto 4.80 g of p-iodo-benzonitrile and then refluxing for 2 hours. After cooling, the product was introduced into iced water, and extracted with hexane. The hexane phase was washed subsequently with water, 1N-HCl aqueous solution and then water, followed by purifying with silica gel column to obtain 5.16 g of oily oa p-(1-trifluoromethyl-heptyloxy)- benzonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05160662 |
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| 出典データセット | uspto-grants-1992_11 |
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| ORD ID | ord-2b8b5b7465ef4adc9b1eda4352119f95 |
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| 出典メモ | uspto-grants-1992_11 |
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