참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3,5-Dichloro-2-cyanopyridine | HCID 2769699 | — |
| 반응물 | Sodium Methoxide | HCID 10942334 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 3-Chloro-5-methoxypicolinonitrile | HCID 18796864 | — |
반응 단계
To a solution of 3,5-dichloropicolinonitrile (1.0 eq.) in dimethyl formamide (DMF) (0.5 M) was added sodium methoxide (1.5 eq.) and heated to 75° C. After stirring for 14 hours, the reaction was diluted with ethyl acetate and water. The organic layer was washed with saturated aqueous NaHCO3 three times, water twice, dried over anhydrous MgSO4, and concentrated en vacuo. The crude residue was purified by a COMBIFLASH® system (ISCO) using 15% ethyl acetate in hexane to give a mixture of two methoxy regioisomers, one of which was the desired product. The mixture was carried onto the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08895577B2 |
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| 출처 데이터셋 | uspto-grants-2014_11 |
|---|
| ORD ID | ord-644b96ca644b477a93e2eaf644a3f724 |
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| 출처 메모 | uspto-grants-2014_11 |
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