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Acetic Acid → HCID 67467860、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Hydroxy-4-methylcyclohexanone | HCID 28539 | — |
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | HCID 67467860 | HCID 67467860 | 72% |
反応手順
4-Hydroxy-4-methylcyclohexanone (440 mg, 3.43 mmol) was dissolved in 1,2-dichloroethane (15 ml), followed by sequential addition of cyclopropylamine (0.26 ml, 3.78 mmol), NaBH(OAc)3 (1.16 g, 5.49 mmol), and acetic acid (0.20 ml, 3.43 mmol), and then the resulting mixture was stirred at room temperature under nitrogen stream for 20 hours. The resulting reaction liquid was neutralized by addition of 10% aqueous NaOH solution, and extracted with 5% MeOH/MC (15 ml×4). The organic layer was dried over anhydrous sodium sulfate, followed by filtration, concentration, and vacuum drying, to obtain 417 mg of yellow solid (72%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09096571B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-2220842ccbbd4c5480c96cb0cd86947b |
| 出典メモ | uspto-grants-2015_08 |