Nitric Acid → 1-Methyl-6-nitro-2-(propan-2-yl)-5-(trifluoromethyl)-1H-benzimidazole
反応式
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[CH:10]([C:13]1[N:17]([CH3:18])[C:16]2[CH:19]=[CH:20][C:21]([C:23]([F:26])([F:25])[F:24])=[CH:22][C:15]=2[N:14]=1)([CH3:12])[CH3:11].[OH-].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>>[CH:10]([C:13]1[N:17]([CH3:18])[C:16]2[CH:19]=[C:20]([N+:1]([O-:4])=[O:2])[C:21]([C:23]([F:25])([F:26])[F:24])=[CH:22][C:15]=2[N:14]=1)([CH3:12])[CH3:11]参加物
6
実験手順
Slowly add 1.01 g. of 90% nitric acid dissolved in 2.2 ml. of concentrated sulfuric acid to a stirred solution of 3.00 g. of 2-isopropyl-1-methyl-5-trifluoromethylbenzimidazole in 13.2 ml. of concentrated sulfuric at about 5° C. Maintain the reaction at about 5° C for 2 hours. Pour the reaction mixture into 300 ml. of ice water and basify with 26 ml. of 50% sodium hydroxide followed by sodium carbonate. Extract with ether, dry over sodium sulfate and evaporate to dryness. Recrystallize from dichloromethane-hexane, obtaining the product of this example.
後処理
- customat about 5° C
- temperatureMaintain
- customthe reaction at about 5° C for 2 hours
- additionPour the reaction mixture into 300 ml
- extractionExtract with ether
- dry with materialdry over sodium sulfate
- customevaporate to dryness
- customRecrystallize from dichloromethane-hexane
- customobtaining the product of this example
出典と根拠
- ORDレコード
- ord-587e105013884d529c5450908778d9c1
- 出典データセット
- uspto-grants-1976_10
- 特許番号
- US03987182
反応ノート
読み込み中…