関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloro-1,2-propanediol | HCID 7290 | — |
| 反応物 | 1-Dodecanethiol | HCID 8195 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1,2-Dihydroxypropane dodecyl sulfide | HCID 86739775 | — |
反応手順
Approximately 397 g of 50% aqueous sodium hydroxide solution was added dropwise over a period of 7 hours to a solution of n-dodecyl mercaptan (1000g) and 1-chloropropane-2,3-diol (547g) in isopropanol solvent (2000 cc) at ambient temperature. The reaction temperature rose from 21° to 56° C. during the addition. The reaction was refluxed for 5 hours at 80° C. and then filtered hot through paper to remove the precipitated salt. The isopropanol solvent was removed by distillation. The product residue was dissolved in about 4000 cc of toluene and washed with water several times. The toluene solution was dried over magnesium sulfate and filtered through diatomaceous earth. Toluene was removed by high speed rotary evaporation to yield a white solid product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04486323 |
|---|
| 出典データセット | uspto-grants-1984_12 |
|---|
| ORD ID | ord-969c057dd3d9439fa55ffda69fe69457 |
|---|
| 出典メモ | uspto-grants-1984_12 |
|---|