化工社化工社 化学情報印刷レポート · 研究参考用
Hydrazine hydrate (1:1) → Diethyl (2-cyanoethyl)phosphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Diethyl (3-aminopropyl)phosphonate | HCID 78113 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Diethyl (2-cyanoethyl)phosphonate | HCID 82369 | 30% |
反応手順
A mixture of diethyl[3-(N-phthalimido)]propylphosphonate (ex. 5) (3.72 g; 11.4 mmoles), absolute ethanol (46 ml) and hydrazine hydrate (0.78 ml of 98% purity; 15.7 mmoles) is stirred at reflux for 35 min. The mixture is filtered and the solvent is distilled under vacuo. The resulting oil is dissolved in CHCl3 (10 ml) and is filtered again. Solvent removal in vacuo gives a colorless liquid (0.7 g; yield 30%). According to example 4, diethyl 3-aminopropylphosphonate (6) is also obtained from diethyl 2-cyanoethylphosphonate in an analogous fashion followed by vacuum distillation at about 115° C. and 0.18 mbar (yield 80%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08105689B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-24f0fb6e5da7496fbad561c15f729533 |
| 出典メモ | uspto-grants-2012_01 |