関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-Bromo-4-propylbenzene | HCID 136374 | — |
| 反応物 | Methionin AL | HCID 446793 | — |
| 反応物 | 1,4-Dioxaspiro[4.5]decan-8-one | HCID 567415 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 8-(4-Propylphenyl)-1,4-dioxaspiro[4.5]decan-8-ol | HCID 65918128 | 71% |
反応手順
Metal magnesium in an amount of 12 g was suspended in 50 ml of THF under nitrogen gas stream, and a solution prepared by dissolving 100 g of 4-n-propylbromobenzene in 300 ml of THF was added dropwise and stirred at room temperature for 1 hour. A solution prepared by dissolving 78 g of 1,4-cyclohexanedione-monoethylene ketal in 300 ml of THF was added dropwise thereto and stirred at room temperature for 1 hour. After finishing of the reaction, 500 ml of a saturated aqueous solution of ammonium chloride was added and extracted with 500 ml of ethyl acetate. Organic layer was washed with water and dried over anhydrous magnesium sulfate, and the solvent was distilled off under a reduced pressure to obtain 98 g of 1,1-ethylenedioxy-4-hydroxy-4-(4-n-propylphenyl)cyclohexane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05858275 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-135fe795830e4ffa9823ba487f930d22 |
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| 出典メモ | uspto-grants-1999_01 |
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