참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 반응물 | 2-Indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one | HCID 57483780 | — |
| 반응물 | 3'-Amino-2'-hydroxy-biphenyl-3-carboxylic acid hydrobromide | HCID 57483789 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Ethanol | HCID 702 | — |
| 생성물 | HCID 178433790 | HCID 178433790 | 11.4% |
반응 단계
Upon cooling by an ice-salt bath, 3′-amino-2′-hydroxy-biphenyl-3-carboxylic acid hydrobromide 1f (267 mg, 1.16 mmol) was dissolved in 10 mL of hydrochloric acid (1 N) followed by addition of 10 mL of aqueous sodium nitrite (88 mg, 1.28 mmol) and 2-indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one 1i (249 mg, 1.16 mmol). The mixture was adjusted to pH 8 with saturated aqueous sodium bicarbonate, followed by addition of 10 mL of ethanol. The reaction mixture was warmed up to room temperature overnight. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered, dried and recrystallized from methanol to obtain the title compound 2′-hydroxy-3′-[N′-(1-indan-5-yl-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene)-hydrazino]-biphenyl-3-carboxylic acid 1 (60 mg, yield 11.4%) as a yellow solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08367710B2 |
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| 출처 데이터셋 | uspto-grants-2013_02 |
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| ORD ID | ord-2105fbc6d636469d9764cffe984178d2 |
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| 출처 메모 | uspto-grants-2013_02 |
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