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Potassium Hydroxide → HCID 13343963、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4,4'-Thiodiphenol | HCID 17570 | — |
| 反応物 | Dicyclohexano-18-crown-6 | HCID 85955 | — |
| 反応物 | O-Ethyl S-propyl chlorothiophosphate | HCID 11745722 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 13343963 | HCID 13343963 | — |
反応手順
To a 250 ml round bottom flask was added 4,4'-thiodiphenol (4.36 g, 20 mmol), O-ethyl S-n-propyl phosphorochloridothioate (9.12 g, 45 mmol), powdered potassium hydroxide (3.37 g, 60 mmol), dicyclohexano-18-crown-6 (catalytic quantity), and acetonitrile. This mixture was refluxed 14 hours, cooled to room temperature, and the organic soluble fraction decanted from the solids. The organic solution was diluted with ether and successively washed with 4M NaOH (3×100 ml), water (2×50 ml), 5% HCl (1×50 ml), water (2×50 ml), and brine (2×50 ml). After drying (MgSO4) the solution was concentrated under reduced pressure to give a colorless oil (4.8 g, 7.6 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04457922 |
| 出典データセット | uspto-grants-1984_07 |
| ORD ID | ord-fc5b32dd410548f1b4fb89eab4fa1bc5 |
| 出典メモ | uspto-grants-1984_07 |