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Water → 1-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-(Chloromethyl)-1H-benzotriazole | HCID 3328222 | — |
| 反応物 | Sodium sulfide monohydrate | HCID 19906495 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-{[(1H-1,2,3-benzotriazol-1-ylmethyl)sulfanyl]methyl}-1H-1,2,3-benzotriazole | HCID 3766092 | 88% |
反応手順
1-(Chloromethyl)benzotriazole (20.4 g), prepared above, and sodium sulfide monohydrate (14.4 g) in anhydrous ethanol (75 ml) were stirred overnight (20 hours) at room temperature. Water (240 ml) was added to the reaction mixture. The precipitate was filtered, washed with water to remove inorganic salts and dried. Crystallization from ethanol gave 15.6 g (88%) of desired product (Compound 1); m.p. 179°-181° C. (lit. 182°-184° C.). Thin Layer Chromotography in (CHCl3 /Ethyl acetate) showed only one spot.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05298390 |
| 出典データセット | uspto-grants-1994_03 |
| ORD ID | ord-21d61f07ab5e409ea3eec212aa4b057a |
| 出典メモ | uspto-grants-1994_03 |