化工社化工社 化学情報印刷レポート · 研究参考用
Glycidol → 6-(2-Oxiranylmethoxy)[1,2,4]triazolo[4,3-b]pyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Glycidol | HCID 11164 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-[1,2,4]triazolo[4,3-b]pyridazine | HCID 313624 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-Oxiranylmethoxy)[1,2,4]triazolo[4,3-b]pyridazine | HCID 23000316 | 32.8% |
反応手順
12.0 g of 2-oxiranylmethanol and 2.50 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazine were dissolved in 40 ml of N,N-dimethylformamide; under ice cooling, 713 mg of 60% oily sodium hydride was added, followed by stirring at room temperature for 30 minutes. After cold saline was added, the reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1) and dried over magnesium sulfate. After concentration under reduced pressure, the residue was subjected to silica gel column chromatography and eluted with ethyl acetate-methanol (10:1). The desired fraction was collected and concentrated under reduced pressure; the precipitated crystal was washed with diethyl ether and dried to yield 1.02 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-8957a2a462814b4bae3c9e5dff4a92b5 |
| 出典メモ | uspto-grants-2003_08 |