関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-B]pyridazin-3-amine | HCID 58045804 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 溶媒 | (+)-2-Butanol | HCID 444683 | — |
| 生成物 | 6-((S)-sec-Butoxy)-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine | HCID 58045871 | — |
反応手順
(S)-Butan-2-ol (1.7 ml) was initially charged at RT with stirring and cooled almost to 0° C. with an ice bath. Subsequently, the mixture was admixed with portions of sodium hydride (85 mg). The suspension formed was heated to 55° C. for 1.5 h and then admixed with portions of 6-chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine (W2.006a, 100 mg), suspended in (S)-butan-2-ol (2 ml) and DMF (2 ml). After stirring at 55° C. for 1 h, the mixture was admixed with water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. 105 mg of the title compound were isolated in sufficient purity. LC-MS rt: 0.81 min [M+H]+: 236.2 (met. b)
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-6c173fa28594464d8c15baef95fe3844 |
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| 出典メモ | uspto-grants-2011_12 |
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