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Benzoyl isothiocyanate → N-Benzoyl-N'-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1,3,4-thiadiazole-2,5-diamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoyl isothiocyanate | HCID 68284 | — |
| 反応物 | N-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-hydrazine carbothioamide | HCID 13657332 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-Benzoyl-N'-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-1,3,4-thiadiazole-2,5-diamine | HCID 13657364 | — |
反応手順
0.33 g (2 mmol) of benzoyl isothiocyanate are added to 0.68 g (2 mmol) of N-[2-hydroxy-3-[3-(1-piperidinylmethyl)phenoxy]propyl]-hydrazine carbothioamide in 20 ml of THF and the reaction mixture is stirred overnight at room temperature. After removal of the THF by evaporation, the solid residue is washed with ether and dissolved in 30 ml of ethanol with heating, and 1 ml of 30% hydrogen peroxide is added. The sulphur which separates is filtered off, the filtrate is concentrated by evaporation and the oily residue is purified by preparative layer chromotography.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727081 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-9e8a6fca991c4f188febdba8ae9ce0c8 |
| 出典メモ | uspto-grants-1988_02 |