N-bromobutanimide → 4-Bromo-7-methoxy-3-methyl-2-trifluoromethylbenzimidazole

HRID 275794

反応式

HRID 275794 の反応式
[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]=1

参加物

4

反応物 2

HCID 67184N-bromobutanimideHCID 183166367-Methoxy-3-methyl-2-trifluoromethylbenzimidazole

生成物 1

HCID 183166224-Bromo-7-methoxy-3-methyl-2-trifluoromethylbenzimidazole収率 92%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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).

後処理

  1. customwas quenched by the addition of 5% sodium metabisulphite solution (50 ml)
  2. customthe organic layer was separated
  3. washWashing with water (50 ml)
  4. dry with materialdrying over anhydrous magnesium sulphate and removal of the solvent in vacuo
  5. customgave an orange oil
  6. customPurification by flash chromatography
  7. washeluting with 50% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-de379988852f45a1b9e7d4a9df08a5f3
出典データセット
uspto-grants-2002_03
特許番号
US06353010B1

関連ノート

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