関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Iodo-4-nitrobenzene | HCID 12495 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 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-Trifluoromethylheptyloxy)nitrobenzene | HCID 15123947 | — |
反応手順
Into 200 ml of dry DMF containing 2.0 g of sodium hydride (purity 60%), were added dropwise 9.2 g of S-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 S-form oa 1-trifluoromethyl-heptanol. After the addition was over, stirring was continued further an hour at room temperature, followed by adding thereto 12.4 g of p-iodo-nitro-benzene 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-hydrochloric acid aqueous solution and then water, followed by purifying with silica gell column to obtain 7.7 g of oily oa p-(1-trifluoromethylheptyloxy)- nitrobenzene.
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-cf72626921c74d82b46ed2443b5116fd |
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| 出典メモ | uspto-grants-1992_11 |
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