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Glycolic Acid → (6-Phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Glycolic Acid | HCID 757 | — |
| 反応物 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 反応物 | 3-Hydrazinyl-6-phenylpyridazine | HCID 6409842 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (6-Phenyl-[1,2,4]triazolo[4,3-b]pyridazin-3-yl)methanol | HCID 57812703 | — |
反応手順
A mixture of 1-(6-phenylpyridazin-3-yl)hydrazine (2.00 g, 10.7 mmol), glycolic acid (0.825 g, 10.8 mmol), p-TsOH.H2O (2.55 g, 13.4 mmol) in PhMe (50 mL) was refluxed for 14 h. PhMe was removed in vacuo. The resulting solids were diluted with water (30 mL). The mixture was brought to pH˜10 with 2N NaOH. The solids were isolated solid by filtration, washed with water and dried under vacuum to give an off white solid which was used without further purification. (ESI, pos. ion) m/z: 227.0 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08524900B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-6989f4bd20934af588a402f67981da7d |
| 出典メモ | uspto-grants-2013_09 |