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Hydrochloric Acid → Octamoxin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium cyanoborohydride | HCID 5003444 | — |
| 反応物 | tert-Butyl N'-(1-methyl-heptylidene)-hydrazinecarboxylate | HCID 72599198 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Octamoxin | HCID 20811 | — |
反応手順
74.08 g (305.7 mmol) of tert-butyl N′-(1-methyl-heptylidene)-hydrazinecarboxylate are dissolved in a mixture of 235 ml of THF and 310 ml of methanol and, after 22.34 g (354.6 mmol) of sodium cyanoborohydride have been added, the mixture is stirred for 1 hour at room temperature. 213 ml of 6N HCl are added dropwise and, after the addition has ended, the mixture is refluxed for 1.5 hours. It is neutralized with 6N NaOH solution, then, after the non-aqueous solvents have been removed, extracted three times with dichloromethane, and, after the mixture has been dried over sodium sulphate, the solvent is removed in vacuo. This gives 37.5 g (85%) of a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06174884B1 |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-9bb64b2018d74f30935863ff29605f87 |
| 出典メモ | uspto-grants-2001_01 |