참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Aldoxime | HCID 7863 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1-(3,5-Dichloropyridin-2-yl)ethanone | HCID 21712163 | — |
| 용매 | Dimethyl Sulfoxide | HCID 679 | — |
| 생성물 | 1-(3-Chloro-5-hydroxypyridin-2-yl)ethanone | HCID 66666961 | 29.1% |
반응 단계
To a solution of 3.8 g of the 1-(3,5-dichloropyridin-2-yl)ethanone prepared in Step 1 in Synthetic Example 2 and 13.8 g of potassium carbonate in 20 ml of dimethylsulfoxide, 5.9 g of acetaldoxime was added, and the mixture was stirred at 80° C. for 4 hours. After completion of the reaction, the reaction mixture was allowed to cool to room temperature, mixed with 50 ml of water and washed with diethyl ether (30 ml×1), the resulting aqueous layer was acidified with 6N aqueous hydrochloric acid and extracted with ethyl acetate (25 ml×2). The resulting organic layers were combined, dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain 1.0 g of desired crude product as brown crystals. The crystals were used in the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09434684B2 |
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| 출처 데이터셋 | uspto-grants-2016_09 |
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| ORD ID | ord-158a104ff5c14a359c477122e58f77c9 |
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| 출처 메모 | uspto-grants-2016_09 |
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