참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Bromoethanol | HCID 10898 | — |
| 반응물 | 3,5-Dimethyl-4-nitropyrazole | HCID 146172 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(3,5-dimethyl-4-nitro-1H-pyrazol-1-yl)ethanol | HCID 19616956 | — |
반응 단계
To a solution of 3,5-dimethyl-4-nitro-1H-pyrazole (500 mg, 3.52 mmol) in MeCN (5 mL), Cs2CO3 (1.26 g, 3.87 mmol) and 2-bromoethanol (0.3 mL, 4.21 mmol) was added. The resulting mixture was refluxed (90° C.) for 3 h, then the reaction mixture was allowed to reach rt. The mixture was diluted with DCM, filtered, the filter cake rinsed with DCM and the filtrate concentrated in vacuo. The residue was partitionned between water and EtOAc, the org. layer was separated and the aq. layer was extracted with EtOAc (1×). The combined org. layers were washed with brine, dried (MgSO4), filtered and concentrated in vacuo to yield 2-(3,5-dimethyl-4-nitro-1H-pyrazol-1-yl)ethanol as a white solid. LC-MS conditions A: tR=0.53 min, [M+H]+=186.39.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09303023B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-37e3e9b30d14439aa2e004f5e331caf0 |
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| 출처 메모 | uspto-grants-2016_04 |
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