化工社化工社 化学情報印刷レポート · 研究参考用
Dichloromethane → 5-Chloro-3-(4-nitrophenyl)-1,2,4-thiadiazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Trichloromethanethiol | HCID 6390 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Nitrobenzamidine hydrochloride | HCID 170625 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Chloro-3-(4-nitrophenyl)-1,2,4-thiadiazole | HCID 20216376 | 40.3% |
反応手順
A solution of 75.6 gm of sodium hydroxide in 100 ml of water was added to a stirred mixture of 101.4 gm of p-nitrobenzamidine hydrochloride, 70 gm of perchloromethyl mercaptan and 760 ml of dichloromethane, while keeping the temperature below -5° C. After additional 2 hours at -5° C., the resulting suspension was filtered, and the organic phase was separated, evaporated to dryness, and the residual solid was recrystallized from 95% ethanol, yielding 45 gm of the title compound, m.p. 143°-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04548944 |
| 出典データセット | uspto-grants-1985_10 |
| ORD ID | ord-b56a310b0915491a95f79994ff1d025a |
| 出典メモ | uspto-grants-1985_10 |