関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Butylate | HCID 16181 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 反応物 | 4-(1,4-Dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane | HCID 21308588 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | HCID 178505689 | HCID 178505689 | 97.3% |
反応手順
23.7 g of potassium t.-butylate were added to a solution of 125.3 g of 4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)-cyclohexane (cis/trans 50/47) in 630 ml of dimethyl sulphoxide, the mixture was stirred at 100° C. for 2 hrs., cooled and poured into 2500 ml of 5 percent sodium chloride solution. The reaction mixture was extracted with methylene chloride, the organic phase was dried over sodium sulfate, filtered and the filtrate was evaporated. Crystallization of the residue from isopropanol gave 121.9 g of trans-4-(1,4-dioxaspiro[4,5]dec-8-yl)-1-(3-fluorophenyl)cyclohexane as colorless crystals (trans content 99.8%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05888423 |
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| 出典データセット | uspto-grants-1999_03 |
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| ORD ID | ord-5ec8769642e9475c888caa24dee08499 |
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| 出典メモ | uspto-grants-1999_03 |
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