반응식
[CH3:1][O:2][C:3]1[C:8]2[N:9]=[C:10]([C:13]([F:16])([F:15])[F:14])[N:11]([CH3:12])[C:7]=2[CH:6]=[CH:5][CH:4]=1.[Br:17]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Br:17][C:6]1[C:7]2[N:11]([CH3:12])[C:10]([C:13]([F:16])([F:14])[F:15])=[N:9][C:8]=2[C:3]([O:2][CH3:1])=[CH:4][CH:5]=1참가 물질
4
실험 절차
To a solution of 7-methoxy-3-methyl-2-trifluoromethylbenzimidazole (1.4 g) in chloroform (50 ml) under nitrogen was added N-bromosuccinimide (1.2 g). The mixture was stirred for 20 minutes before the reaction was quenched by the addition of 5% sodium metabisulphite solution (50 ml) and the organic layer was separated. Washing with water (50 ml), drying over anhydrous magnesium sulphate and removal of the solvent in vacuo gave an orange oil. Purification by flash chromatography eluting with 50% ethyl acetate in hexane gave the title compound as an orange solid (1.73 g).
후처리
- customwas quenched by the addition of 5% sodium metabisulphite solution (50 ml)
- customthe organic layer was separated
- washWashing with water (50 ml)
- dry with materialdrying over anhydrous magnesium sulphate and removal of the solvent in vacuo
- customgave an orange oil
- customPurification by flash chromatography
- washeluting with 50% ethyl acetate in hexane
출처 및 근거
- ORD 기록
- ord-de379988852f45a1b9e7d4a9df08a5f3
- 출처 데이터셋
- uspto-grants-2002_03
- 특허 번호
- US06353010B1
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