Thionyl Chloride → 2-Chloro-1-methyl-5-nitro-1H-benzimidazole
反応式
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]=2[NH:4][C:3]1=S.O=S(Cl)[Cl:17]>>[Cl:17][C:3]1[N:2]([CH3:1])[C:6]2[CH:7]=[CH:8][C:9]([N+:11]([O-:13])=[O:12])=[CH:10][C:5]=2[N:4]=1参加物
3
実験手順
The compound 1-Methyl-5-nitro-1,3-dihydro-benzoimidazole-2-thione (5.8 g, 27.9 mmol) was heated to reflux with SOCl2 (30 ml) overnight. The reaction mixture was cooled to room temperature and poured into 300 ml of ice water and extracted with CH2Cl2. The organic layers was washed with 10% NaHCO3 water solution, brine, dried over Na2SO4 and concentrated to give the title compound as a yellow solid. MS (ESI) m/z=212 [M+H].
後処理
- extractionextracted with CH2Cl2
- washThe organic layers was washed with 10% NaHCO3 water solution, brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-95436be09f304e759035941098a0666d
- 出典データセット
- uspto-grants-2008_03
- 特許番号
- US07338959B2
反応ノート
読み込み中…