Water → 2-Amino-5-bromobenzenemethanol
반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][C:9]=1[C:10](OC)=[O:11].O.[OH-].[Na+]>C1COCC1>[NH2:7][C:8]1[CH:17]=[CH:16][C:15]([Br:18])=[CH:14][C:9]=1[CH2:10][OH:11]참가 물질
6
실험 절차
To a suspension of lithium aluminium hydride (0.33 g, 8.7 mmol) in THF (10 ml) was added a solution of methyl 2-amino-5-bromobenzoate (2.0 g, 8.7 mmol) in 20 ml THF at 0° C. under nitrogen. Then stirring was continued for 2 h. 0.64 ml water, 2 M solution of sodium hydroxide (0.64 ml) and again 1.28 ml water were added before the resulting mixture was filtered through celite. Evaporation of the solvent and purification of the crude product by flash chromatography on silica gel (dichloromethane/ethyl acetate, 2/1) yielded (2-amino-5-bromophenyl)methanol (1.0 g, 5.2 mmol, 59%) as off-white solid.
후처리
- filtrationwas filtered through celite
- customEvaporation of the solvent and purification of the crude product by flash chromatography on silica gel (dichloromethane/ethyl acetate, 2/1)
출처 및 근거
- ORD 기록
- ord-eac0c260257f408f86bcc379c762a4e5
- 출처 데이터셋
- uspto-grants-2013_09
- 특허 번호
- US08541404B2
반응 노트
불러오는 중…