참여 물질
| 역할 | 이름 | HCID | 투입량 |
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| 반응물 | Phosphorus tribromide | HCID 24614 | — |
| 반응물 | (4-Bromo-2,3-difluorophenyl)methanol | HCID 66819962 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 1-Bromo-4-(bromomethyl)-2,3-difluorobenzene | HCID 69672854 | 51.5% |
반응 단계
To a solution of (4-bromo-2,3-difluorophenyl)methanol (500 mg, 2.242 mmol) in DCM (10 mL) stirred under N2 at 0° C. was added PBr3 (0.634 mL, 6.73 mmol) in one charge. The reaction mixture was stirred at 10° C. for 2 h. Then the solution was concentrated and distributed between DCM and saturated NaHCO3 solution. The combined organic extract was washed with brine, dried over MgSO4, filtered and concentrated. The crude material was purified by preparative TLC (PE/EA=10:1, Rf 0.6) to yield light yellow oil of 1-bromo-4-(bromomethyl)-2,3-difluorobenzene (330 mg, 1.154 mmol, 51.5% yield): 1H NMR (400 MHz, CDCl3) δ 7.30 (ddd, J=2.0, 6.0, 8.2 Hz, 1H), 7.11-7.03 (m, 1H), 4.46 (s, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09035063B2 |
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| 출처 데이터셋 | uspto-grants-2015_05 |
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| ORD ID | ord-2bd6f17c4306464487f448038b025aa7 |
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| 출처 메모 | uspto-grants-2015_05 |
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