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Stannane, trimethylphenyl- → 3-Methylthio-5-phenyl-1,2,4-thiadiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Stannane, trimethylphenyl- | HCID 123095 | — |
| 反応物 | Potassium Fluoride | HCID 522689 | — |
| 反応物 | 5-Chloro-3-(methylsulfanyl)-1,2,4-thiadiazole | HCID 570953 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-Methylthio-5-phenyl-1,2,4-thiadiazole | HCID 23086910 | 72.8% |
反応手順
To 30 ml of toluene were added 500 mg of 5-chloro-3-methylthio-1,2,4-thiadiazole, 794 mg of trimethylphenyltin and 346 mg of tetrakistriphenylphosphine palladium, and the mixture was heated under reflux for 8 hours in a nitrogen atmosphere. Then, the reaction mixture was cooled to room temperature, and a 20% aqueous potassium fluoride solution was added to the reaction mixture, followed by stirring. This mixture was filtered through Celite, and the filtrate was concentrated. The resulting residue was subjected to silica gel column chromatography to obtain 455 mg of 3-methylthio-5-phenyl-1,2,4-thiadiazole.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07361675B2 |
| 出典データセット | uspto-grants-2008_04 |
| ORD ID | ord-32428475ae3e40a3b5eaaa00620bcfc6 |
| 出典メモ | uspto-grants-2008_04 |