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 | Formicin | HCID 69365 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | P-((Acetylamino)methyl)phosphonic acid | HCID 3017080 | 154.4% |
反応手順
20 g (0.225 mol) of N-hydroxymethylacetamide were dissolved in 20 ml of acetic acid and cooled to 5° C. under a nitrogen atmosphere and with stirring. 12.4 g (0.113 mol) of diphosphorus trioxide (P2O3) were then added dropwise at 5° to 10° C. with stirring during the course of 20 minutes. The mixture was then stirred without cooling until room temperature was reached. It was then heated to reflux for 31/2 hours. It was then cooled. 2 g (0.11 mol) of water were then added dropwise with stirring, the temperature rising to 35° C. After cooling, the acetic acid was removed under reduced pressure and with continuous warming to 95° C. The crystalline residue was digested with ethanol. 26 g of crude acetylaminomethanephosphonic acid having a melting point of 171°-175° C. were obtained. After recrystallization from 88% strength aqueous acetic acid, 19 g (55% of theory) of acetylaminomethanephosphonic acid having a melting point of 186° to 90° C. were obtained. The CHNP elemental analysis of a sample gave:
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-967f232b82e44e29ab1118de18402754 |
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| 出典メモ | uspto-grants-1992_10 |
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