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Pyridine → Di-(2-ethylthioethyl)2-chloroethanephosphonate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 2-(Ethylthio)ethanol | HCID 8075 | — |
| 反応物 | (2-Chloroethyl)phosphonic dichloride | HCID 69645 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Di-(2-ethylthioethyl)2-chloroethanephosphonate | HCID 85916432 | — |
反応手順
To a solution of 18.1 g (0.1 mol) of 2-chloroethane phosphonic acid dichloride in 150 ml of absolute ether is added dropwise with stirring a solution of 21.2 g (0.2 mol) of hydroxyethyl ethyl sulphide and 15.8 g of absolute pyridine in 100 ml of absolute ether at room temperature, during which the temperature increases to 35° and crystallisation occurs. Stirring is continued for a further 14 hours at 25° after which the crystals are removed by filtration and the ethereal filtrate is washed to neutrality with 5% hydrogen carbonate solution and water. It is dried and evaporated and further dried by rotation under high vacuum for 2 hours. A yellow oil is obtained having the following characterisation data:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04190430 |
| 出典データセット | uspto-grants-1980_02 |
| ORD ID | ord-13e9384b72ff4f8c82a8c6f56f8594b2 |
| 出典メモ | uspto-grants-1980_02 |