참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 1,10-Phenanthroline | HCID 1318 | — |
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | Methyl 3-iodo-5-nitrobenzoate | HCID 7020599 | — |
| 반응물 | HCID 178428601 | HCID 178428601 | — |
| 촉매 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | 3-(4-Methyl-2-oxo-2H-pyridin-1-yl)-5-nitro-benzoic acid methyl ester | HCID 57851325 | 99.9% |
반응 단계
To a 25 ml round-bottomed flask was added 2-Hydroxy-4-methylpyridine (17.9 mg, 0.164 mmol), 3-Iodo-5-nitro-benzoic acid methyl ester (40 mg, 0.137 mmol), CuI (5.2 mg, 0.027 mmol) and 1,4-dioxane (10 ml). The reaction mixture was stirred for 5 minutes to the dissolve 2-Hydroxy-4-methylpyridine and 3-iodo-5-nitro-benzoic acid methyl ester, after which 1,10-phenanthroline (9.84 mg, 0.055 mmol) was added, followed by K3PO4 (174 mg, 0.082 mmol). The reaction mixture was flushed with N2, and heated to 110° C. for 24 hours. After cooling to room temperature, the mixture was diluted with H2O, and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by flash chromatography to give 3-(4-Methyl-2-oxo-2H-pyridin-1-yl)-5-nitro-benzoic acid methyl ester (39.45 mg, 61%) as light yellow solid. MS (M+H)=289.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08846945B2 |
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| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-abc31ea669f04fa9b7f70a3f3681bc8e |
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| 출처 메모 | uspto-grants-2014_09 |
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