関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Morpholinomethylphosphonic acid | HCID 4491459 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Glyphosate | HCID 3496 | 34.1% |
| 生成物 | (Aminomethyl)phosphonic acid | HCID 14017 | 31.5% |
反応手順
To a 100 mL Monel autoclave were added 2.23 g (12.3 mmol) of 4-morpholinylmethylphosphonic acid 7.88 g (98.5 mmol) of a 50% solution of NaOH, and 10 mL of H2O to give a slurry. The vessel was flushed with N2, sealed and heated to 250° C. This temperature was maintained for five and one-half hours with little noticeable reaction occurring. The temperature was then raised to 300° C. for three hours. During this period the internal pressure in the vessel rose from 4.5×106N/M2 to 5.7×106N/M2. The vessel was cooled to room temperature and the residual pressure was released. The resulting solution was diluted with water and neutralized with 8.1 mL (98.5 mmol) of conc. HCl. The solution was concentrated to dryness. The residue was taken up in conc. HCl and the precipitated NaCl was filtered away. The final filtrate was concentrated and purified by ion exchange chromatography to yield 0.71 g (34.1 %) of N-phosphonomethylglycine and 0.43 g (31.5%) of aminomethylphosphonic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04587061 |
|---|
| 出典データセット | uspto-grants-1986_05 |
|---|
| ORD ID | ord-c3b15df5d8db42b38dddb3d173cb23dd |
|---|
| 出典メモ | uspto-grants-1986_05 |
|---|