関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | ethyl phosphonothioic dichloride, anhydrous | HCID 61246 | — |
| 反応物 | 3-Sulfanylbutan-1-ol | HCID 6430893 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Ethyl-1,3,2-oxathiaphosphepane 2-sulphide | HCID 20185070 | 59% |
反応手順
16.3 g (0.1 mol) of ethanethiophosphonic dichloride in 1 l of toluene are initially introduced, and a mixture of 11 g (0.1 mol) of 3-mercaptobutan-1-ol and 22 g (0.22 mol) of triethylamine in 100 ml of tetrahydrofuran is slowly added dropwise at 20° C. The mixture is heated at 80° C. for 2 days, and 200 ml of toluene and 200 ml of water are then added to the reaction mixture. The organic phase is separated off, washed with water and dried, and the solvent is distilled off, first under a vacuum from a waterpump and then under a high vacuum. 11.5 g (59 % of theory) of 2-ethyl-1,3,2-oxathiaphosphepane 2-sulphide having a refractive index nD20 =1.5761 are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04695563 |
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| 出典データセット | uspto-grants-1987_09 |
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| ORD ID | ord-af85d24e43d14ffea4997d3637857b2d |
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| 出典メモ | uspto-grants-1987_09 |
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