참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 3-(Dimethylamino)-1-phenyl-2-propen-1-one | HCID 353460 | — |
| 반응물 | HCID 178418806 | HCID 178418806 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 생성물 | 7-Phenylpyrazolo[1,5-a]pyrimidine | HCID 20033008 | — |
반응 단계
A reaction mixture of 5.25 g. of 3-dimethylaminoacrylophenone [von H. Meerwein et al., Annalen der Chemie, Band 641, 1-39, (1961)] and 2.50 g. of 3-aminopyrazole in 25 ml. of glacial acetic acid is refluxed for 3.5 hours, cooled overnight and evaporated to a thick yellow oil. This oil is dissolved in methylene chloride, washed with a saturated aqueous solution of sodium bicarbonate, dried over sodium sulfate and then passed through a sintered glass funnel or a chromatographic column packed in vacuo with hydrous magnesium silicate. Additional methylene chloride is passed through the funnel (column). The effluent is refluxed on a steam bath. The gradual addition of hexane produces crystals. The crystallization from methylene chloride with hexane is repeated giving the desired product, m.p. 72°-73° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US04236005 |
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| 출처 데이터셋 | uspto-grants-1980_11 |
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| ORD ID | ord-3dfd30dd07e440e58fbc082d3833cd5e |
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| 출처 메모 | uspto-grants-1980_11 |
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