참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 6-Chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-B]pyridazin-3-amine | HCID 58045804 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | (+)-2-Butanol | HCID 444683 | — |
| 생성물 | 6-((S)-sec-Butoxy)-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine | HCID 58045871 | — |
반응 단계
(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)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08076336B2 |
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| 출처 데이터셋 | uspto-grants-2011_12 |
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| ORD ID | ord-6c173fa28594464d8c15baef95fe3844 |
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| 출처 메모 | uspto-grants-2011_12 |
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