참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 반응물 | 3,6-Dichloro-4-methylpyridazine | HCID 87923 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | 6-Chloro-3-hydrazinyl-4-methylpyridazine | HCID 11446490 | 39.1% |
반응 단계
3,6-Dichloro-4-methylpyridazine (Combi-Blocks) (60 g, 361 mmol) was dissolved in hydrazine monohydrate (Aldrich) (335 mL, 5411 mmol) and the solution was stirred at 80° C. for 1 h, forming a white precipitate. The reaction mixture is dilutes with water and the precipitated products isolated by filtration. The solid crude product is suspended in EtOH and left in an ultra sound bath for 1 h. The desired product (22.4 g) was obtained after filtration and drying under vacuum as a beige solid. tR: 0.31 min (LC-MS 2); ESI-MS: 160.0 [M+H]+ (LC-MS 2). 1H NMR (400 MHz; DMSO-d6) δ ppm 7.83 (br.s, 1H) 7.32 (s, 1H) 4.49 (br.s, 2H) 2.05 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08975417B2 |
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| 출처 데이터셋 | uspto-grants-2015_03 |
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| ORD ID | ord-cb3edca2b4dd4f3fab854d9cc4acc786 |
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| 출처 메모 | uspto-grants-2015_03 |
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