참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Phenoxyethanol | HCID 31236 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 반응물 | HCID 178507967 | HCID 178507967 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-(2-phenoxyethoxy)-1H-pyrazol-5-amine | HCID 18981597 | 33% |
반응 단계
There was suspended, in 2-phenoxy ethanol (25 g, 180 mM), 5-amino-1H-pyrazol-3-ol (4.00 g, 41.4 mM), then p-toluenesulfonic acid monohydrate (15.4 g, 80.8 mM) was added to the suspension and the mixture was stirred at 130° C. for 5 hours under reduced pressure. This reaction liquid was diluted with acetonitrile, the solid precipitated out of the liquid was filtered off and washed with acetonitrile. The resulting solid was suspended in a 6% aqueous sodium bicarbonate solution (250 mL), the suspension was stirred at room temperature and the solid was then filtered off. The resulting solid was dissolved in ethyl acetate, dried over anhydrous sodium sulfate and then the solvent was distilled off to thus give the title compound (2.90 g, yield: 33%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08314098B2 |
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| 출처 데이터셋 | uspto-grants-2012_11 |
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| ORD ID | ord-19d64cded8924a4db4d3cb715631a67a |
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| 출처 메모 | uspto-grants-2012_11 |
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