참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Methyl 3-amino-4-bromobenzoate | HCID 3928639 | — |
| 촉매 | Zinc cyanide (Zn(CN)2) | HCID 11186 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 생성물 | Methyl 3-amino-4-cyanobenzoate | HCID 10261604 | 94% |
반응 단계
Add zinc cyanide (1.5 g, 12.77 mmol), palladium tetrakis (675 mg, 0.584 mmol), to 3-amino-4-bromo-benzoic acid methyl ester (1.328 g, 5.77 mmol) in anhydrous DMF (3 ml). Purge with nitrogen for few minutes and keep under nitrogen atmosphere while heating to 120° C. overnight. Cool the mixture to room temperature and add water. Extract the product with EtOAc (×2). Wash the combined organic layers with 2N ammonium hydroxide solution (×2), water (×2), saturated aq. sodium chloride and dry over anhydrous sodium sulfate, filter and concentrate to yield the crude product. Purification by flash chromatography (Silica gel-hexane/EtOAc) yields 3-amino-4-cyano-benzoic acid methyl ester (94%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07393868B2 |
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| 출처 데이터셋 | uspto-grants-2008_07 |
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| ORD ID | ord-00f200ac29324156975343ac5dc5cd6b |
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| 출처 메모 | uspto-grants-2008_07 |
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