참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Butyl vinyl ether | HCID 8108 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 1,3-Bis(diphenylphosphino)propane | HCID 81219 | — |
| 반응물 | 3-(4-Chlorophenyl)-7-hydroxy-8-iodo-2-isopropyl-chromen-4-one | HCID 59724246 | — |
| 촉매 | palladium(II) acetate | HCID 167845 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 8-Acetyl-3-(4-chlorophenyl)-7-hydroxy-2-isopropyl-chromen-4-one | HCID 59724269 | — |
반응 단계
3-(4-Chlorophenyl)-7-hydroxy-8-iodo-2-isopropyl-chromen-4-one (1.1 g, 2.5 mmol), 1,3-bis(diphenylphosphino)propane (206 mg, 0.5 mmol), palladium acetate (56 mg, 0.25 mmol) and potassium carbonate (380 mg, 2.75 mmol) are mixed in N-methyl-2-pyrrolidinone (10 ml) in a 20 ml capacity microwave tube. Water (2 ml) and butyl vinyl ether (1.62 ml, 12.5 mmol) are added, the tube is sealed, and the mixture is heated at 80° C. under microwave irradiation for 45 min. The mixture is cooled to room temperature, poured into water (30 ml) and extracted with ethyl acetate (3×50 ml). The ethyl acetate extracts are combined, washed with saturated brine (50 ml), dried (MgSO4), filtered and evaporated to give a brown solid. This is purified by chromatography on silica gel using cyclohexane/ethyl acetate (6:1) as eluant to give a colourless solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07732435B2 |
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| 출처 데이터셋 | uspto-grants-2010_06 |
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| ORD ID | ord-1f7d75009f3e45e8b5f63eb1176a7c1f |
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| 출처 메모 | uspto-grants-2010_06 |
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