関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Phosphorus trioxide | HCID 14810 | — |
| 反応物 | N-(hydroxymethyl)benzamide | HCID 80493 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | Benzoylaminomethanephosphonic acid | HCID 10443251 | 132.5% |
反応手順
11 g (0.1 mol) of diphosphorus trioxide (P2O3) were dissolved in 70 ml of tetrahydrofuran and the solution was cooled to 5° C. 30.2 g (0.2 mol) of N-hydroxymethylbenzamide were then added in portions at 5°-10° C. in the course of 30 minutes with stirring and under a nitrogen atmosphere. The mixture was then allowed to come to room temperature with stirring and was then heated to reflux for 2 hours; a clear solution was not formed in this case. After cooling to room temperature, 4.5 g (0.25 mol) of water were added dropwise at 30°-40° C. and the mixture was then heated to reflux for 1 hour. It was then cooled, additionally stirred and filtered with suction. 28.5 g of benzoylaminomethanephosphonic acid having a melting point of 171° to 173° C. were obtained. A further 5 g were isolated from the mother liquor. Altogether, 33.5 g (78% of theory) of product were thus obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05155257 |
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| 出典データセット | uspto-grants-1992_10 |
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| ORD ID | ord-0d7cb84140024d548a7036ce74597bae |
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| 出典メモ | uspto-grants-1992_10 |
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