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Acetic Acid → 3-(Hydroxyamino)propylphosphonic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Methane | HCID 297 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | diethyl 3-(N-benzyloxy-N-tosylamino)propylphosphonate | HCID 20337228 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-(Hydroxyamino)propylphosphonic acid | HCID 342170 | 51.2% |
反応手順
A mixture of diethyl 3-(N-benzyloxy-N-tosylamino)propylphosphonate (13.2 g), conc. hydrochloric acid (130 ml) and acetic acid (130 ml) was refluxed with stirring for 45 hours. The resultant mixture was concentrated under reduced pressure to give a residue and then water and an activated charcoal was added thereto, whereafter the mixture was filtered. The filtrate was concentrated under reduced pressure, and the resultant residual oil (8.59 g) was dissolved in water (25 ml). To the solution were added pyridine (2.08 g) and ethanol (5 ml), and then the mixture was allowed to stand overnight at 4° C. to give 3-(N-hydroxyamino)propylphosphonic acid (2.30 g) in the form of crystals. MP: 160°-166° C. (dec.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04206156 |
| 出典データセット | uspto-grants-1980_06 |
| ORD ID | ord-7ebae7d6fe9a4b51b45084ab10a6e6cf |
| 出典メモ | uspto-grants-1980_06 |