関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Nitrocyclohexane | HCID 14285 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 19705663 | HCID 19705663 | — |
反応手順
A ethanol (5 mL) solution of nitrocyclohexane (5.00 g, 38.7 mmol) and sodium hydroxide (12.5 g, 0.3 mmol) was heated to 55° C., 35% formalin solution (3.0 mL, 35 mmol) was added, and the mixture was heated and stirred at the same temperature for 1.5 hours. The reaction mixture was diluted with water, 2M hydrochloric acid (0.5 mL, 1 mmol) was added, and the mixture was extracted with ethyl acetate (15 mL) two times. The organic layer was washed with 5% sodium bicarbonate aqueous solution (10 mL) and water (20 mL), and then dried with anhydrous sodium sulfate. The solvents were removed by distillation under reduced pressure, the residue was refined with silica gel column chromatography (Highflash 3L, manufactured by Yamazen Corporation, the mixture of hexane and ethyl acetate of 3:1 in mixing ratio), and colorless oily (1-nitro-cyclohexyl)-methanol (6.96 g) was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08367666B2 |
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| 出典データセット | uspto-grants-2013_02 |
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| ORD ID | ord-74b7df4c55644a818119d13f6e7b8b2a |
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| 出典メモ | uspto-grants-2013_02 |
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