化工社化工社 化学情報印刷レポート · 研究参考用
Water → 6-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one | HCID 6407182 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Chloro-2-triphenylmethyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one | HCID 23000307 | 71.6% |
反応手順
0.341 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one and 0.669 g of chlorotriphenylmethane were dissolved in 5 ml of N,N-dimethylformamide; 0.414 ml of N-ethyldiisopropylamine was added, followed by stirring at room temperature for 2 days. After water was added, the reaction mixture was extracted with ethyl acetate; the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with hexane-ethyl acetate (2:1). The desired fraction was collected and concentrated; the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.591 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06610694B1 |
| 出典データセット | uspto-grants-2003_08 |
| ORD ID | ord-fbbef0e461ac4f1bafb5463b640ff18f |
| 出典メモ | uspto-grants-2003_08 |