참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Anhydride | HCID 7918 | — |
| 반응물 | Isoamyl Nitrite | HCID 8053 | — |
| 반응물 | Potassium Acetate | HCID 517044 | — |
| 반응물 | 4-(Acetylamino)-2,5-dimethylphenyl acetate | HCID 19078613 | — |
| 촉매 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-acetyl-6-methyl-1H-indazol-5-yl acetate | HCID 69430758 | 46% |
반응 단계
Acetic anhydride (0.96 ml, 10.2 mmol), tetrabutylammonium bromide (55 mg, 0.169 mmol), potassium acetate (665 mg, 6.78 mmol) and isoamyl nitrite (0.592 ml, 4.41 mmol) were added to a solution of 4-(acetylamino)-2,5-dimethylphenyl acetate (750 mg, 3.39 mmol) in ethyl acetate (7.5 ml) at room temperature, and the resulting mixture was refluxed. After 9 hours, the reaction solution was poured into water (50 ml) and extracted with ethyl acetate (50 ml×2), and the organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 1-acetyl-6-methyl-1H-indazol-5-yl acetate (359 mg, 46%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07199147B2 |
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| 출처 데이터셋 | uspto-grants-2007_04 |
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| ORD ID | ord-3617566acb644d40b8982d67857f84d5 |
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| 출처 메모 | uspto-grants-2007_04 |
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