참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methanol | HCID 887 | — |
| 반응물 | Nitrogen | HCID 947 | — |
| 반응물 | 2-Chloro-4-cyanopyridine | HCID 568638 | — |
| 용매 | Dioxane Methanol | HCID 21966525 | — |
| 생성물 | 2-Methoxyisonicotinonitrile | HCID 7204887 | — |
반응 단계
Under a stream of N2 and with cooling, Na metal (2.7 g) was added to MeOH (36 ml) with a considerable exotherm. After the Na is dissolved, a solution of 2-chloro-4-cyanopyridine (15 g) in dioxane:MeOH (1:1, 110 ml) was added via dropping funnel over a 10 min period. The reaction was heated to reflux for 3.5 h then cooled at ˜10° C. overnight. Solid was filtered off and the solid was washed with MeOH. The filtrate was concentrated to ˜60 ml and H2O (60 ml) was added to redissolve a precipitate. Upon further concentration, a precipitate formed which was washed with H2O. Further concentration produced additional solids. The solids were combined and dried in vacuo overnight at 35° C. to provide 4-cyano-2-methoxypyridine which was used as is.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08642624B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-64dfeb30f56d4b0999f61d5d123fd063 |
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| 출처 메모 | uspto-grants-2014_02 |
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