化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 3,5-Dimethyl-4-sulfanylphenol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3,5-Dimethylphenol | HCID 7948 | — |
| 反応物 | Dimethyl Disulfide | HCID 12232 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 反応物 | CID 15930840 | HCID 15930840 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 3,5-Dimethyl-4-sulfanylphenol | HCID 14547459 | 93% |
反応手順
61 grams (0.5 mole) of 3,5-xylenol dissolved in 250 cc glyme was added to 67 grams (0.5 mole) of sulfur monochloride dissolved in 200 cc glyme at room temperature. The temperature rose immediately to about 50° C. After 2 minutes, the reaction mixture was poured into 2400 grams of an aqueous solution of about 227 grams (3.4 moles) of sodium methyl mercaptide and 217 grams (5.4 moles) of sodium hydroxide. The mixture was then heated to its boiling point. After the glyme and dimethyl disulfide had boiled off, the mixture was acidified with concentrated hydrochloric acid to precipitate a pale yellow oil which crystallized rapidly to a colorless solid. A 93% yield of 4-mercapto-3,5-xylenol was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04056568 |
| 出典データセット | uspto-grants-1977_11 |
| ORD ID | ord-4dcda43804e745e389134870905dc2fa |
| 出典メモ | uspto-grants-1977_11 |