Phosphorus tribromide → 1-(Bromomethyl)-3-chloro-2-methylbenzene
반응식
P(Br)(Br)[Br:2].[Cl:5][C:6]1[C:7]([CH3:14])=[C:8]([CH2:12]O)[CH:9]=[CH:10][CH:11]=1>C1(C)C=CC=CC=1>[Br:2][CH2:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:6]([Cl:5])[C:7]=1[CH3:14]참가 물질
4
실험 절차
To a solution of phosphorus tribromide (0.422 mL, 4.47 mmol) in Toluene (30 mL) was added (3-chloro-2-methylphenyl)methanol (2 g, 12.77 mmol). The reaction was stirred at RT overnight. The solvent was removed and the residue was partitioned between EtOAc and brine. The organic layer was concentrated and the residue was purified by biotage (5% EA/hexane) to give the product (2.0 g, 71%). 1H NMR (400 MHz, CDCl3) δppm 7.36 (m, 1H), 7.24 (m, 1H), 7.12 (m, 1H), 4.56 (s, 2H). 2.48 (s, 3H).
후처리
- customThe solvent was removed
- customthe residue was partitioned between EtOAc and brine
- concentrationThe organic layer was concentrated
- customthe residue was purified by biotage (5% EA/hexane)
출처 및 근거
- ORD 기록
- ord-bb8c0663e90045979d612542183e75cd
- 출처 데이터셋
- uspto-grants-2013_04
- 특허 번호
- US08410095B2
반응 노트
불러오는 중…