関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phosphonic acid | HCID 407 | — |
| 反応物 | 2-Pyrrolidone | HCID 12025 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Azacyclopentane-2,2-diphosphonic acid | HCID 12886166 | — |
反応手順
85.0 gm of 2-pyrrolidone (1.0 mol) and 164 gm of H3PO3 (2.0 mols) were melted at 80°C. While stirring this melt, 176 ml of PCl3 (2.0 mols) were added thereto. The mixture was stirred for three additional hours and was left standing at 70°C overnight. Then, three liters of H2O were used for the hydrolysis. The solution was boiled with activated carbon; and after filtration, the reaction product was precipitated with acetone. The white substance was dissolved in water, and passed over a cation exchanger. The solution was concentrated; and the substance was separated upon the addition of ethanol. The yield of crystalline azacyclopentane-2,2-diphosphonic acid was 95 gm, or about 41% of the theory. The molecular weight of the compound was determined by titration to be 230 (calculated: 231.09).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03941772 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-c5f3f267239c41feab5f273d047f417b |
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| 出典メモ | uspto-grants-1976_03 |
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