참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | Sodium Bromide | HCID 253881 | — |
| 반응물 | Cyclopropylboronic acid | HCID 2760897 | — |
| 반응물 | 5-Bromo-1,3-difluoro-2-nitrobenzene | HCID 21335487 | — |
| 촉매 | HCID 178418397 | HCID 178418397 | — |
| 용매 | Toluene | HCID 1140 | — |
| 생성물 | 5-Cyclopropyl-1,3-difluoro-2-nitrobenzene | HCID 59683254 | 141% |
반응 단계
5-bromo-1,3-difluoro-2-nitrobenzene (D24, 560 mg, 2.35 mmol), cyclopropylboronic acid (1 eq., 2.35 mmol, 0.2 g), K3PO4 (3 eq., 7.1 mmol, 1.50 g), NaBr (1 eq., 2.35 mmol, 0.24 g) and Pd(PPh3)4 (280 mg) were added to 3 ml of dry toluene and the mixture was heated by microwave at 160° C. for 40 minutes. The mixture was then poured onto water (10 ml) and extracted with ethyl acetate (3×20 ml). The combined organics were dried over MgSO4, filtered and the solvent was evaporated to afford 660 mg of brown crude product which was purified by silica gel chromatography (5-20% diethyl ether-40-60° petroleum ether) to afford the title compound as a yellow oil, 300 mg, 64%.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08481566B2 |
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| 출처 데이터셋 | uspto-grants-2013_07 |
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| ORD ID | ord-562985611e7a4cdeaa8c4734b214ebe1 |
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| 출처 메모 | uspto-grants-2013_07 |
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