関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfide | HCID 1068 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Chlorosuccinimide | HCID 31398 | — |
| 反応物 | 2,4,5-Trifluoroaniline | HCID 94953 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 2-Methylthiomethyl-3,4,6-trifluoroaniline | HCID 18974461 | — |
反応手順
To 2,4,5-trifluoroaniline (35.0 g) are added anhydrous dichloromethane (530 ml) and dimethyl sulfide (24.6 ml) and the mixture is cooled to 0° C. Thereto N-chlorosuccinimide (38.2 g) is gradually added below 5° C. After the mixture is stirred at the same temperature for 15 minutes, triethylamine (47.7 ml) is gradually added. After reflux for 12 hours, the resultant is made alkaline with 5% aqueous sodium hydroxide solution, extracted with dichloromethane, and the extract is dried over sodium sulfate and concentrated. The residue is purified with column chlomatography (silica-gel, dichloromethane: n-hexane=1:4) to give 2-methylthiomethyl-3,4,6-trifluoroaniline (22.3 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05723648 |
|---|
| 出典データセット | uspto-grants-1998_03 |
|---|
| ORD ID | ord-dd7b84cd2bdd41c8acecfbb08583d7c0 |
|---|
| 出典メモ | uspto-grants-1998_03 |
|---|