참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 4-Chloro-2-iodophenol | HCID 620234 | — |
| 반응물 | tert-butyl 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate | HCID 16217654 | — |
| 촉매 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | tert-butyl 4-(5-chloro-2-hydroxyphenyl)-1H-pyrazole-1-carboxylate | HCID 59436518 | 66% |
반응 단계
A suspension of 4-chloro-2-iodophenol (200 mg, 0.78 mmol) and potassium carbonate (434 mg, 3.14 mmol) in 1,4-dioxane (3 mL) and water (1 mL) was degassed and heated for 1 hour at 50° C. tert-Butyl 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole-1-carboxylate (347 mg, 1.18 mmol) and palladium (0) tetrakis(triphenylphoshine) (91 mg, 0.08 mmol) were added and the mixture heated at 50° C. for 5 hours. Dichloromethane (20 ml) and water (10 ml) were added and the organics separated and evaporated in vacuo. The residue was purified by column chromatography (silica gel) eluting with ethyl acetate:heptane (2:8 to 1:0, by volume) to afford the title product as a white solid, 155 mg, 66% yield.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08541588B2 |
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| 출처 데이터셋 | uspto-grants-2013_09 |
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| ORD ID | ord-49e6dad53c78479fad1a4142b9f5c63e |
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| 출처 메모 | uspto-grants-2013_09 |
|---|