化工社化工社 化学情報印刷レポート · 研究参考用
Trichloromethanesulfenyl chloride → 5-Chloro 3-(2,4,6-trimethylphenyl)1,2,4-thiadiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trichloromethanesulfenyl chloride | HCID 11666 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Mesitylformamidin | HCID 18788461 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 5-Chloro 3-(2,4,6-trimethylphenyl)1,2,4-thiadiazole | HCID 18788458 | 99.1% |
反応手順
2.2 g of trichloromethanesulfenyl chloride are introduced into a solution of 2 g of 2,4,6-trimethyl benzamidine in 16 ml of dichloromethane under an inert atmosphere at about -20° C., followed by the slow addition of 2 g of NaOH dissolved in 3.2 ml of water at about -10° C. After I hour at about -5° C., the precipitate formed is isolated and the organic phase is separated and washed with 6 ml of water. After being dried over K2CO3, it is concentrated under reduced pressure to give 2.8 g of the desired product in the form of an oil, which may be used without purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05470855 |
| 出典データセット | uspto-grants-1995_11 |
| ORD ID | ord-80152b1af913426387206ec895462f2e |
| 出典メモ | uspto-grants-1995_11 |