참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Azide | HCID 33558 | — |
| 반응물 | 2,3-Dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid hydrazide | HCID 12790239 | — |
| 반응물 | 2,3-Dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid azide monohydrochloride | HCID 12797519 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-amino-6-(4-pyridinyl)-3(2H)-pyridazinone | HCID 12790240 | — |
반응 단계
The above procedure of Example G-1 first procedes through the acid azide as seen by the following isolation of the acid azide as its monohydrochloride: To a solution chilled in an ice bath and containing 3.0 g. of 2,3-dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid hydrazide and 60 ml. of 6 N hydrochloric acid was added dropwise with stirring a solution containing 3.0 g. of sodium nitrite in 10 ml. of water over a 30 minute period. The reaction mixture was then stirred for an additional 1 hour, allowing the reaction mixture to warm up to room temperature. The separated solid was collected, washed with water and dried in a vacuum oven over P2O5 at 25° C. for 48 hours to yield 3.0 g. of 2,3-dihydro-3-oxo-6-(4-pyridinyl)-4-pyridazinecarboxylic acid azide monohydrochloride, m.p. >300° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04346221 |
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| 출처 데이터셋 | uspto-grants-1982_08 |
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| ORD ID | ord-61b597167197461d9dc9e6fb0ce0906e |
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| 출처 메모 | uspto-grants-1982_08 |
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