참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Sodium ethoxide | HCID 2723922 | — |
| 반응물 | 6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine trifluoroacetate | HCID 86650795 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 6-Ethoxy-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine | HCID 58045920 | 83.2% |
반응 단계
6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine trifluoroacetate (W2.002b; 50 mg) was dissolved in ethanol (3.5 ml) while stirring at RT. Thereafter, sodium ethoxide was added dropwise while cooling with ice (25 mg dissolved in 1.5 ml of ethanol). After stirring at RT for 2.5 h, the mixture was heated to 60° C. and, after 2.5 h, a further equivalent of sodium ethoxide solution was added. After standing overnight, the mixture was heated again to 60° C., two further equivalents of sodium ethoxide solution were added and the mixture was stirred for 4 h. Subsequently, 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. 27 mg of the title compound were obtained. LC-MS rt: 0.67 min [M+H]+: 194.1 (met. a)
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09079906B2 |
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| 출처 데이터셋 | uspto-grants-2015_07 |
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| ORD ID | ord-b5f99ce73b1d4dbf9a103da46b418b24 |
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| 출처 메모 | uspto-grants-2015_07 |
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