関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dabco | HCID 9237 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | O,O-diethyl phosphorochloridothioate | HCID 17305 | — |
| 反応物 | boric acid, sodium salt | HCID 159383 | — |
| 反応物 | Sodium 3,5,6-trichloropyridinate | HCID 23699972 | — |
| 触媒 | Benzyl triethylammonium chloride | HCID 66133 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Chlorpyrifos | HCID 2730 | 97% |
反応手順
O,O-Diethyl phosphorochloridothioate (11.3 g., 0.06 mole) was added dropwise to a stirred mixture of (1) sodium 3,5,6-trichloro-2-pyridinate (13.2 g., .06 mole) in 30 ml. of methylene chloride and 74 ml. of water, (2) 1 mole percent triethylene diamine, (3) 1 mole percent benzyltriethylammonium chloride and (4) a pH buffer consisting of NaOH and sodium borate. The stirred reaction mixture was maintained at 42° C. for 1.5 hours, cooled to room temperature, and the organic phase separated from the aqueous phase. The organic phase was washed once with approximately 30 ml. water and the organic solvent removed under reduced pressure. The title compound was thus obtained in 97 percent yield, based on 100 percent conversion of starting materials. The product was of excellent purity (approximately 99% pure).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04016225 |
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| 出典データセット | uspto-grants-1977_04 |
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| ORD ID | ord-3cd95343a7914640b2cc6a3c20f9eb5b |
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| 出典メモ | uspto-grants-1977_04 |
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