참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Diethylamine | HCID 8021 | — |
| 반응물 | 6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide | HCID 86650796 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N6,n6-diethyl-8-methyl-1,2,4-triazolo[4,3-b]pyridazine-3,6-diamine | HCID 58136920 | — |
반응 단계
6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.002; 250 mg) was dissolved in abs. DMF (2 ml) and admixed with diethylamine (7 ml). Thereafter, the reaction mixture was placed into a heating block at 80° C. with stirring for 11 days. The solvent was then drawn off and the residue was admixed with a little water and extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate, filtered and concentrated. The residue was purified by means of preparative HPLC (met. A), and the clean product fractions were combined, freed of the acetonitrile under reduced pressure, alkalized with saturated potassium carbonate solution and extracted repeatedly with dichloromethane. The combined organic phases were dried over sodium sulfate, filtered and concentrated. 100 mg of the title compound were obtained.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08198272B2 |
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| 출처 데이터셋 | uspto-grants-2012_06 |
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| ORD ID | ord-3a65638af6fd48d88d2ea7b7ca94b982 |
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| 출처 메모 | uspto-grants-2012_06 |
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