참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Ethyl Acetate | HCID 8857 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 5-Formamido-1-methylpyrazole | HCID 2755869 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 5-(N-formyl-N-methylamino)-1-methylpyrazole | HCID 22916760 | — |
반응 단계
To a solution of 5-formamido-1-methylpyrazole in N,N-dimethylformamide (50 ml) was sodium hydride (1.6 g) under ice-cooling. Then, to the mixture was added methyl iodide (2.5 ml) at the same condition. The mixture was stirred for 1 hour under ice-cooling. To the reaction mixture was added a mixture of ethyl acetate (500 ml) and water (100 ml). The organic layer was separated, and the aqueous layer was extracted with ethyl acetate (50 ml×2). The organic solution was dried over magnesium sulfate. The solvent was distilled off and the residue was subjected to a column chromatography on silica gel using a mixture of ethyl acetate and diisopropyl ether (3:1) as an eluent. Fractions containing the object compound were collected and evaporated in vacuo to give 5-(N-formyl-N-methylamino)-1-methylpyrazole (2.5 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05663163 |
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| 출처 데이터셋 | uspto-grants-1997_09 |
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| ORD ID | ord-ea9e1aaa7a704baeb11b1cd0521584d0 |
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| 출처 메모 | uspto-grants-1997_09 |
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