Lithium Bromide → 1-(2-Bromo-ethoxymethyl)-4-chlorobenzene
반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][O:7][CH2:8][CH2:9]OS(C)(=O)=O)=[CH:4][CH:3]=1.[Br-:17].[Li+]>CC(C)=O>[Br:17][CH2:9][CH2:8][O:7][CH2:6][C:5]1[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=1참가 물질
4
실험 절차
A mixture of methanesulfonic acid 2-(4-chloro-benzyloxy)-ethyl ester (Intermediate 6) (1.37 g, 5.18 mmol) and lithium bromide (1.80 g, 20.7 mmol) in acetone (15 mL) was heated at reflux overnight. The reaction mixture was concentrated to dryness and the residue partitioned between DCM and water. The organic layer was dried (MgSO4), and concentrated, and purified by column chromatography over silica using DCM/cyclohexane (1:3) as eluent to afford the product as a colourless oil.
후처리
- temperaturewas heated
- temperatureat reflux overnight
- concentrationThe reaction mixture was concentrated to dryness
- customthe residue partitioned between DCM and water
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated
- custompurified by column chromatography over silica
출처 및 근거
- ORD 기록
- ord-59ca3905a1594c12915c5fbac4032272
- 출처 데이터셋
- uspto-grants-2010_12
- 특허 번호
- US07846955B2
반응 노트
불러오는 중…