関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,3-Dimethoxy-2-propanol | HCID 12190 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide | HCID 86650796 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-(2-Methoxy-1-methoxymethylethoxy)-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine | HCID 58045905 | — |
反応手順
1,3-Dimethoxypropan-2-ol (12.96 ml) was initially charged in DMF (25 ml), admixed under argon with sodium hydride (681 mg) and stirred at 40° C. for 1 h. Subsequently, 6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.002; 1.5 g), dissolved in DMF (25 ml), was added dropwise within 20 min. After 1 h, the mixture was admixed with water and extracted by shaking four times with dichloromethane. The combined organic phases were dried over magnesium sulfate and concentrated by rotary evaporation. The residue was triturated with MtB ether, filtered off with suction and dried. 764 mg of the title compound were isolated. LC-MS rt: 0.74 min [M+H]+: 268.1 (met. a)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08076336B2 |
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| 出典データセット | uspto-grants-2011_12 |
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| ORD ID | ord-fbede180588444a09ed2d48ec861c335 |
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| 出典メモ | uspto-grants-2011_12 |
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