Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Phosphorus tribromide → 2-Benzyloxy-5-bromomethyl-1,3-dichloro-benzene
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Phosphorus tribromide | HCID 24614 | — |
| 반응물 | (4-Benzyloxy-3,5-dichlorophenyl)methanol | HCID 16749116 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-Benzyloxy-5-bromomethyl-1,3-dichloro-benzene | HCID 16749117 | — |
반응 단계
Phosphorous tribromide (2 mL) was added to a solution of (4-benzyloxy-3,5-dichloro-phenyl)-methanol (CAB02117, 5.50 g, 19.4 mmol) in dichloromethane (80 mL) at 0° C. The mixture was stirred at this temperature for 2 h, diluted with diethyl ether (150 mL), transferred into a separation funnel and washed with water (2×50 mL) and brine (50 mL). The organic layer was dried over magnesium sulphate and concentrated under reduced pressure. The residue was recrystallised from dichloromethane/hexane. 1H-NMR (400 MHz, CDCl3) δ 4.39 (s, 2H, —CH12Br), 5.05 (s, 2H, —CH2Ph), 7.37 (s, 2H), 7.38-7.44 (m, 3H), 7.54-7.58 (m, 2H). 13C-NMR (100 MHz, CDCl3) δ=31.48, 75.39, 128.73, 129.68, 129.70, 129.72, 130.06, 135.46, 136.27, 151.23.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07745472B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-061a6b08f971414da70dc59bc14b4c14 |
| 출처 메모 | uspto-grants-2010_06 |