참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Chloroform | HCID 6212 | — |
| 반응물 | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| 반응물 | 2-Amino-4-methyl-3-nitropyridine | HCID 243166 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Cyclopropanecarboxamido-4-methyl-3-nitropyridine | HCID 15380885 | 75% |
반응 단계
A mixture comprising 5.0 g (32.6 mmol) of 2-amino-4-methyl-3-nitropyridine and 5.2 g of pyridine was heated at 110° C. in a nitrogen atmosphere. 3.8 g (36 mmol) of cyclopropanecarbonyl chloride was dropwise added thereto, followed by further stirring at 110° C. for 5 hours. The reaction mixture was brought to room temperature, followed by the addition of chloroform (50 ml) and water (50 ml). The organic phase was separated and the aqueous phase was further extracted with chloroform (50 ml) twice. The organic phases were combined and washed with water (20 ml) and a saturated aqueous solution (20 ml) of common salt, successively. The resultant organic phase was dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel column chromatography (a n-hexane/ethyl acetate system) to give 5.4 g of the title compound (yield 75%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05618969 |
|---|
| 출처 데이터셋 | uspto-grants-1997_04 |
|---|
| ORD ID | ord-43b59089586343c4a28a2d609750b65f |
|---|
| 출처 메모 | uspto-grants-1997_04 |
|---|