참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridazine | HCID 9259 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | hydroxylamine-O-sulfonic acid | HCID 76284 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | N-aminopyridazinium sulfate | HCID 69698706 | — |
반응 단계
A solution of hydroxylamine-O-sulfonic acid (73.4 g) in water (80 mL) and a separate solution of potassium carbonate (65.5 g) in water (80 mL) were added concurrently dropwise to a solution of pyridazine (40.0 g) in water (120 mL) at 50° C., maintaining a reaction mixture pH of 3.5-4.0. The reaction mixture was then heated at 40° C. for 2 hours to give a solution of N-aminopyridazinium sulfate, which was subsequently cooled to 20° C. and filtered. The filtrate was added dropwise to a solution of potassium hexafluorophosphate (91.9 g) in water (460 mL) at 50° C. The resulting suspension was slowly cooled to 5° C. over a 2 hour period, stirred for 30 minutes and the product isolated by filtration. The filtercake was washed portionwise with water (320 mL) and the product dried in vacuo at 40° C. to give the title compound as a white crystalline solid (69.9 g, 58%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06803463B2 |
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| 출처 데이터셋 | uspto-grants-2004_10 |
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| ORD ID | ord-7fc5ab3d86a64735ad38223e8198a70f |
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| 출처 메모 | uspto-grants-2004_10 |
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