참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Phenelzine Sulfate | HCID 61100 | — |
| 반응물 | 3-Oxo-3-(pyridin-2-yl)propanenitrile | HCID 11571823 | — |
| 반응물 | Dichloromethane methanol | HCID 21226129 | — |
| 용매 | Ethanol | HCID 702 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 2-Phenethyl-5-pyridin-2-yl-2H-pyrazol-3-ylamine | HCID 67299908 | — |
반응 단계
To a stirred solution of 3-oxo-3-pyridin-2-yl-propionitrile (0.46 g, 3.1 mmol; CAS 54123-21-6) at r.t. in EtOH (10 ml) under an argon atmosphere were added triethylamine (2.6 ml, 18.9 mmol) and phenelzine sulfate salt (2.2 g, 9.4 mmol). The mixture was heated to reflux and stirring was continued for 2 hrs. The orange solution was cooled to r.t. The solids were filtered off. The filtrate was concentrated to leave an orange viscous oil which was taken up in EtOAc and washed with water. The aqueous layer was extracted with EtOAc and with CH2Cl2/MeOH 9:1. The combined organics were dried over MgSO4, filtered and concentrated. The product was obtained after silica gel chromatography using CH2Cl2/MeOH as gradient as off-white solid (0.722 g, 87%). MS: M=265.1 (M+H)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08470820B2 |
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| 출처 데이터셋 | uspto-grants-2013_06 |
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| ORD ID | ord-3345add7cd204414b6fe60d36c6e73b3 |
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| 출처 메모 | uspto-grants-2013_06 |
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