関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Phenylacetaldehyde | HCID 998 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Cyclohexane | HCID 8078 | — |
| 反応物 | 2,3-Dimercaptopropane | HCID 61217 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 20398674 | HCID 20398674 | — |
反応手順
Into a 100 cc reaction flask equipped with reflux condenser, magnetic stirring bar and thermometer and hot plate equipped with magnetic stirring apparatus is placed 5 ml cyclohexane, 0.2 grams of para-toluenesulfonic acid and 5.4 grams (0.05 moles) of 1,2-propanedithiol. With stirring, over a period of 30 minutes, 6 grams (0.05 moles) of phenylacetaldehyde is added to the reaction mass. The reaction mass is then heated to reflux and refluxed for a period of 8 hours. During the refluxing period, water of reaction is removed. At the end of the refluxing period, the reaction mass is cooled to room temperature and transferred to a separatory funnel. The reaction mass is then washed with one 50 ml portion of saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and filtered. The resulting filtrate is distilled on a Microvigreux column yielding the following three fractions:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04515968 |
|---|
| 出典データセット | uspto-grants-1985_05 |
|---|
| ORD ID | ord-b2aec404a6724b75be1cceecbe7a91ce |
|---|
| 出典メモ | uspto-grants-1985_05 |
|---|